1 |
石灰氮一次性水解的工艺方法 |
CN201610665703.5 |
2016-08-13 |
CN106278948A |
2017-01-04 |
王先武; 钱潮涌; 金斐; 王利平; 张飞 |
本发明公开了石灰氮一次性水解的工艺方法,主要包括:(1)向水解釜中投入石灰氮和水,再从水解釜底部缓慢通入气体二氧化碳,控制温度在26-35℃,反应过程中随时监测水解釜内的pH,控制PH值在8-9;(2)将步骤1中所有物料通过压滤机进行压滤,压滤后的滤液即为液态单氰胺钙盐,再将其抽至胺化釜,向胺化釜里滴加氯甲酸甲酯,不断搅拌,即可合成氰胺基甲酸甲酯钙盐。本发明通过一次性水解降低甲酯消耗,消除危险固废,减少二氧化碳排放,甲酯消耗降低10%以上,酯化釜效率增加2倍。 |
2 |
新的羟肟酸衍生物 |
CN96194830.2 |
1996-03-29 |
CN1187810A |
1998-07-15 |
桐尾佳惠; 前田贵子; 佐佐木则雄; 外岛德重; 泽井伸光; 布鲁斯·米利根; 约瑟夫·佩雷斯; 让-彼埃尔·沃尔斯; 丹尼尔·B·甘特 |
通式(Ⅰ)的羟肟酸衍生物,其中G是下式的G1或G2或G3或G4:R5OC=C(COOR4)-、R5ON=C(COOR4)-、R5ON=C(CONR6R7)、R5OC=C(CONR6R7)-,X1、X2、X3是H、卤素、HO、巯基、硝基、SCN、叠氮基、CN、烷基、卤代烷基、氰基烷基、烷氧基、卤代烷氧基、氰基烷氧基、烷基硫代、卤代烷基硫代、氰基烷基硫代、烷基亚磺酰基、卤代烷基亚磺酰基、烷基磺酰基、卤代烷基磺酰基、环烷基、卤代环烷基、烯基、炔基、烯氧基、炔氧基、烯基硫代、炔基硫代、氨基、烷基氨基、二烷基氨基、酰基氨基、烷氧羰基、N-烷基氨基甲酰基、N,N-二烷基氨基甲酰基、N-烷基氨磺酰基、N,N-二烷基氨磺酰基,R1、R2是H或烷基、卤代烷基、环烷基、卤代环烷基、氰基、烷氧基烷基、烷氧基羰基;或R1和R2可以在一起形成二价基团,R3是H或烷基、卤代烷基、环烷基、卤代环烷基、烯基、炔基、烷氧基烷基、烷基硫代烷基、氰基烷基、卤代烷氧基烷基、二烷基氨基烷基、任选取代的苯基、任选取代的苄基,W是O、S、SO或SO2,R4、R5是烷基,R6、R7是H或烷基。 |
3 |
一种环合剂N-(甲氧基羰基)亚氨基甲酸二甲酯及利用该环合剂合成芬苯达唑的方法 |
CN202310767018.3 |
2023-06-27 |
CN116496181A |
2023-07-28 |
潘鹏; 程贺; 樊竹叶 |
本发明公开了一种环合剂N‑(甲氧基羰基)亚氨基甲酸二甲酯及利用该环合剂合成芬苯达唑的方法,涉及芬苯达唑及其中间体的制备技术领域,亚氨基碳酸二甲酯在碱催化作用下失去质子,增加了N原子的亲核能力,与氯甲酸甲酯接触时,N原子进攻羰基碳,形成中间体,后氯原子在钠离子作用下从中间体中脱落,得到环合剂N‑(甲氧基羰基)亚氨基甲酸二甲酯,用环合剂N‑(甲氧基羰基)亚氨基甲酸二甲酯与4‑苯硫基邻苯二胺反应,得到的芬苯达唑,反应过程中避免使用过多的有机溶剂及有机碱,有效降低了生产成本,环合剂N‑(甲氧基羰基)亚氨基甲酸二甲酯生产过程中只产生钠盐,不产生铵盐,降低了后期的处理成本和处理难度,对环境友好。 |
4 |
一种N-氰亚胺碳酸二酯的合成方法 |
CN201510289901.1 |
2015-05-29 |
CN104860848B |
2016-03-09 |
马向东; 黄伟; 杨毅跃 |
一种N-氰亚胺碳酸二酯的合成方法,包括以下步骤:(1)四氯化碳与碱金属醇化合物发生亲核取代反应,生成二氯二氧烷基甲烷、一氯三氧烷基甲烷或四氧烷基甲烷;(2)N-氰亚胺碳酸二酯粗品制备:二氯二氧烷基甲烷在碱性条件下与单氰胺反应生成N-氰亚胺碳酸二酯和氯化物,或者一氯三氧烷基甲烷在碱性条件下与单氰胺反应生成N-氰亚胺碳酸二酯和氯化物,或者四氧烷基甲烷在碱性条件下与单氰胺反应生成N-氰亚胺碳酸二酯;(3)N-氰胺碳酸二酯粗品精制。本发明与现有N-氰胺碳酸二酯的生产工艺相比,摒弃了使用氯气、氰化物等剧毒原辅料,而且工艺操作简单、环境友好,适合大规模工业化生产。 |
5 |
一种石灰氮一次性水解的工艺 |
CN201510325122.2 |
2015-06-11 |
CN104961655A |
2015-10-07 |
袁晓林; 储兵兵; 陈建平; 李永华; 吴双齐; 查日飞; 高焰兵 |
本发明提供了一种石灰氮一次性水解的工艺,首先在水解反应釜内添加石灰氮,同时向水解反应釜内不断通入含有氮气和二氧化碳混合气体,再向水解反应釜内滴加质量比为1~2:1的水和浓度为5-15%的甲醇溶液,此时釜内的PH值为6.5-6.8,不断搅拌。本发明采用单氰胺生产技术,使得石灰氮一次水解得以实现,由于提供了高品质的氰胺液,在滴氰胺基甲酸甲酯的过程中可减少氰胺基甲酸甲酯的滴入量,降低了消耗,为连续化生产打好基础;极大的提高了水解釜的效率,减少了压滤机的工作时间,降低了甲酯的消耗,为氢氰胺基液的生产提高了连续生产的可行,甲酯消耗降低5%以上,酯化釜效率增加1.5倍。 |
6 |
一种环合剂N-(甲氧基羰基)亚氨基碳酸二甲酯及利用该环合剂合成芬苯达唑的方法 |
CN202310767018.3 |
2023-06-27 |
CN116496181B |
2023-09-01 |
潘鹏; 程贺; 樊竹叶 |
本发明公开了一种环合剂N‑(甲氧基羰基)亚氨基碳酸二甲酯及利用该环合剂合成芬苯达唑的方法,涉及芬苯达唑及其中间体的制备技术领域,亚氨基碳酸二甲酯在碱催化作用下失去质子,增加了N原子的亲核能力,与氯甲酸甲酯接触时,N原子进攻羰基碳,形成中间体,后氯原子在钠离子作用下从中间体中脱落,得到环合剂N‑(甲氧基羰基)亚氨基碳酸二甲酯,用环合剂N‑(甲氧基羰基)亚氨基碳酸二甲酯与4‑苯硫基邻苯二胺反应,得到的芬苯达唑,反应过程中避免使用过多的有机溶剂及有机碱,有效降低了生产成本,环合剂N‑(甲氧基羰基)亚氨基碳酸二甲酯生产过程中只产生钠盐,不产生铵盐,降低了后期的处理成本和处理难度,对环境友好。 |
7 |
一种石灰氮一次性水解的工艺 |
CN201510325122.2 |
2015-06-11 |
CN104961655B |
2017-01-18 |
袁晓林; 储兵兵; 陈建平; 李永华; 吴双齐; 查日飞; 高焰兵 |
本发明提供了一种石灰氮一次性水解的工艺,首先在水解反应釜内添加石灰氮,同时向水解反应釜内不断通入含有氮气和二氧化碳混合气体,再向水解反应釜内滴加质量比为1~2:1的水和浓度为5-15%的甲醇溶液,此时釜内的PH值为6.5-6.8,不断搅拌。本发明采用单氰胺生产技术,使得石灰氮一次水解得以实现,由于提供了高品质的氰胺液,在滴氰胺基甲酸甲酯的过程中可减少氰胺基甲酸甲酯的滴入量,降低了消耗,为连续化生产打好基础;极大的提高了水解釜的效率,减少了压滤机的工作时间,降低了甲酯的消耗,为氢氰胺基液的生产提高了连续生产的可行,甲酯消耗降低5%以上,酯化釜效率增加1.5倍。 |
8 |
一种N-氰亚胺碳酸二酯的合成方法 |
CN201510289901.1 |
2015-05-29 |
CN104860848A |
2015-08-26 |
马向东; 黄伟; 杨毅跃 |
一种N-氰亚胺碳酸二酯的合成方法,包括以下步骤:(1)四氯化碳与碱金属醇化合物发生亲核取代反应,生成二氯二氧烷基甲烷、一氯三氧烷基甲烷或四氧烷基甲烷;(2)N-氰亚胺碳酸二酯粗品制备:二氯二氧烷基甲烷在碱性条件下与单氰胺反应生成N-氰亚胺碳酸二酯和氯化物,或者一氯三氧烷基甲烷在碱性条件下与单氰胺反应生成N-氰亚胺碳酸二酯和氯化物,或者四氧烷基甲烷在碱性条件下与单氰胺反应生成N-氰亚胺碳酸二酯;(3)N-氰胺碳酸二酯粗品精制。本发明与现有N-氰胺碳酸二酯的生产工艺相比,摒弃了使用氯气、氰化物等剧毒原辅料,而且工艺操作简单、环境友好,适合大规模工业化生产。 |
9 |
制备2-烷氧基-6-(三氟甲基)嘧啶-4-酚的方法 |
CN200710181206.9 |
2004-02-02 |
CN101255125A |
2008-09-03 |
比特·施米特; 劳伦特·达克里; 麦克尔·戈特施波纳; 布鲁诺·里特内尔 |
本申请涉及制备2-烷氧基-6-(三氟甲基)嘧啶-4-酚的方法。制备下式III的亚氨碳酸二烷基酯的方法,其中R1、R2为C1-C8烷基,包括使氯化氰C1-CN与至少一种其中R是R1或R2的C1-C8醇ROH反应的步骤,并且其中醇包括悬浮形式的固体氢氧化物。 |
10 |
海绵动物抗肿瘤化合物 |
CN01809444.9 |
2001-03-20 |
CN1429203A |
2003-07-09 |
田中淳一; 比嘉辰雄 |
分离自海绵动物的新抗肿瘤化合物,如式(1)、(2)、(3)和(4)所示。 |
11 |
New fluorinated alkoxy imines and their N-chloro- and
N-bromo-derivatives, and process for their preparation |
US677173 |
1991-03-29 |
US5118844A |
1992-06-02 |
Darryl D. Desmarteau; Stefan P. Kotun |
The present invention relates to novel fluorinated alkoxyimines having the formula:R.sub.x --CF.dbd.N--O--CZ.sub.1 Z.sub.2 --CF.sub.3 (I)wherein:R.sub.x is either F or a perhalogenated alkyl group containing from 1 to 3 carbon atoms, andZ.sub.1 and Z.sub.2, either equal to, or different from, each other, are F, Cl, Br, H or a perfluorinated alkyl group containing from 1 to 3 carbon atoms.They are prepared by reacting a fluorinated alkoxyamine haivng the formula:R.sub.x --CF.sub.2 --NH--O--CZ.sub.1 Z.sub.2 --CF.sub.3 (V)with KF at a temperature comprised within the range of from 0.degree. C. to 100.degree. C.The present invention relates furthermore to the N-chloro- and N-bromo-derivatives of said fluorinated alkoxyimines (I), which derivatives have the formulae:R.sub.x --CF.sub.2 --NCl--O--CZ.sub.1 Z.sub.2 CF.sub.3 (VII)andR.sub.x --CF.sub.2 --NBr--O--CZ.sub.1 Z.sub.2 --CF.sub.3 (VIII). |
12 |
Preparation of dialkyl (N-cyanoimido)carbonates from dialkyl
imidocarbonates and cyanogen halides |
US823518 |
1992-01-21 |
US5237084A |
1993-08-17 |
Michael A. Oliver; Ward H. Oliver |
Dialkyl (N-cyanoimido) carbonates are prepared in good yield in a non-aqueous solvent by a process which comprises either (a) adding a cyanogen halide at a controlled rate to a reactor containing an unsubstituted or substituted dialkyl imidocarbonate, an inorganic base and/or a trialkyl amine, or (b) by adding a trialkyl amine to a solution of the unsubstituted or substituted dialkyl imidocarbonate and a cyanogen halide. The dialkyl imidocarbonate precursors are prepared by using a stoichiometric ratio (2:1) of alcohol to cyanogen halide in the presence of an acid acceptor and in a non-aqueous solvent.Dialkyl (N-cyanoimido)carbonates are useful as intermediates for pesticides and pharmaceuticals. |
13 |
Fluorinated alkoxyimines and their N-chloro- and N-bromo-derivatives,
and process for their preparation |
US692960 |
1991-04-26 |
US5081299A |
1992-01-14 |
Darryl D. DesMarteau; Stefan P. Kotun |
Novel fluorinated alkoxy imines having the formula:R.sub.x --CF.dbd.N--O--CZ.sub.1 Z.sub.2 --CF.sub.3 (I)wherein:R.sub.x is either F or a perhalogenated alkyl group containing from 1 to 3 carbon atoms, andZ.sub.1 and Z.sub.2, either equal to, or different from, each other, are F, C1, Br, H or a perfluorinated alkyl group containing 1 to 3 carbon atoms. They are prepared by reacting a fluorinated alkoxy-amine having the formula:R.sub.x --CF.sub.2 --NH--O--CZ.sub.1 Z.sub.2 --CF.sub.3 (V)with Kf at a temperature within the range of from 0.degree. to 100.degree. C. Furthermore, N-chloro- and N-bromo-derivatives of said fluorinated alkoxy-imines (I) are provided, which derivatives have the formulae:R.sub.x --CF.sub.2 --NCl--O--CZ.sub.1 Z.sub.2 --CF.sub.3 (VII)andR.sub.x --CF.sub.2 --NBr--O--CZ.sub.1 Z.sub.2 --CF.sub.3 (VIII) |
14 |
Preparation of fungicidal quinazolinones and useful intermediates |
US202394 |
1998-12-09 |
US6166208A |
2000-12-26 |
James Francis Bereznak; Eric Allen Marshall; Charlene Gross Sternberg; Jeffrey Arthur Sternberg; King-Mo Sun |
This invention provides advantageous processes for preparing quinazolinones of Formula I ##STR1## wherein: R.sup.1 is C.sub.1 -C.sub.10 alkyl; C.sub.3 -C.sub.10 alkenyl; C.sub.3 -C.sub.10 cycloalkyl; C.sub.3 -C.sub.10 halocycloalkyl; C.sub.4 -C.sub.10 cycloalkylalkyl; C.sub.4 -C.sub.10 halocycloalkylalkyl; or C.sub.3 -C.sub.10 alkynyl;R.sup.2 is C.sub.1 -C.sub.10 alkyl; C.sub.3 -C.sub.10 alkenyl; C.sub.3 -C.sub.10 cycloalkyl; C.sub.3 -C.sub.10 halocycloalkyl; C.sub.4 -C.sub.10 cycloalkylalkyl; C.sub.4 -C.sub.10 halocycloalkylalkyl; C.sub.4 -C.sub.10 cycloalkyl; C.sub.4 -C.sub.10 halocycloalkyl; or C.sub.3 -C.sub.10 alkynyl; andR.sup.3 and R.sup.4 are each independently hydrogen or halogen; from compounds containing the moiety IIg ##STR2## This invention further provides certain compounds of Formula II, IIIa, or IVa ##STR3## where R.sup.7 is C.sub.2 -C.sub.6 alkyl. |
15 |
Process for the preparation of N-cyanoimidocarbonates |
US914268 |
1992-07-15 |
US5208351A |
1993-05-04 |
Franz Thalhammer; Stefan Weiss |
The present invention provides a process for the preparation of N-cyanoimidocarbonates of the general formula: ##STR1## in which R.sup.1 and R.sup.2 are the same and are alkyl radicals containing up to 4 carbon atoms or R.sup.1 and R.sup.2 are joined together to give an ethylene or propylene chain which is optionally substituted by an alkyl radical containing up to 3 carbon atoms, wherein an imidocarbonate obtained in aqueous alkaline solution from the appropriate alcohol and cyanogen chloride is added with an acid to an aqueous solution of cyanamide in such a manner that the reaction mixture has a pH value of from 3 to 8. |
16 |
Sponge anti-tumor compounds |
JP2001568888 |
2001-03-20 |
JP2003528075A |
2003-09-24 |
辰雄 比嘉; 淳一 田中 |
(57)【要約】 海綿より単離された、新規な抗腫瘍化合物は、下式(1)、(2)、(3)、及び(4): 【化1】 |
17 |
Production method of N- cyan imide carbonate |
JP18912092 |
1992-07-16 |
JP3162488B2 |
2001-04-25 |
ヴァイス シュテファン; タールハンマー フランツ |
|
18 |
Preparation of dialkyl (n-cyanoimido)carbonate |
JP18633692 |
1992-06-19 |
JPH05186412A |
1993-07-27 |
MAIKERU EE ORIBUAA; UOODO EICHI ORIBUAA |
PURPOSE: To obtain a dialkyl (N-cyanoimido)carbonate useful as an intermediate of a pesticide or pharmaceuticals with a high yield in a nonaq. solvent system in which the isolation (extraction) of an intermediate product is not necessary without using expensive unstable cyanamide.
CONSTITUTION: A cyanogen halide, preferably cyanogen chloride or cyanogen bromide is allowed to react with an optionally substd. dialkyl imidocarbonate, preferably a compd. of formula I (wherein R
1 and R
2 are each a 1-6C alkyl, etc., which may have a substituent such as a 1-3C alkoxy, etc., preferably 1-3C alkyl) at -20 to +40°C, preferably -10 to +10°C in a nonaq. solvent, preferably tert. butyl methyl ether, THF, acetone or methylene chloride in the presence of a catalytic amt. of a trialkylamine, preferably trimethylamine or triethylamine and an inorg. salt, preferably an alkali metallic carbonate. The objective optionally substd. dialkyl (N-cyanoimido)carbonate, preferably a compd. of formula II is advantageously obtd.
COPYRIGHT: (C)1993,JPO |
19 |
Method of manufacturing a dialkyl (n- cyanoimido) carbonate |
JP18633692 |
1992-06-19 |
JP3165871B2 |
2001-05-14 |
エイチ. オリヴァー ウォード; エー. オリヴァー マイケル |
|
20 |
JPH0579665B2 - |
JP6026684 |
1984-03-27 |
JPH0579665B2 |
1993-11-04 |
TOMIOKA HIROKI; OOISHI TADASHI; TAKAHASHI JUNYA; SASAKI MITSURU; HIRATA NAONORI |
|