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A one-pot process for preparing 3-(2,2,2-trimethylhydrazinium)propionate dihydrate

A technology of dihydrate and trimethylhydrazine, applied in the preparation of hydrazine, organic chemistry, etc., can solve the problems of the standard alkali hydrolysis of carbonates and sulfates, etc., and achieve the effect of increasing yield and high yield

Inactive Publication Date: 2013-06-12
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Standard alkaline hydrolysis of carbonates and sulfates (at 3- (2,2,2-trimethylhydrazinium)propionate salts (in the case of alkyl-3-(2,2,2-trimethylhydrazinium) propionate salts)

Method used

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  • A one-pot process for preparing 3-(2,2,2-trimethylhydrazinium)propionate dihydrate
  • A one-pot process for preparing 3-(2,2,2-trimethylhydrazinium)propionate dihydrate
  • A one-pot process for preparing 3-(2,2,2-trimethylhydrazinium)propionate dihydrate

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Effect test

Embodiment 1

[0018] Preparation of 3-(2,2,2-trimethylhydrazine)propionate dihydrate

[0019] Dissolve methyl 3-(2,2-dimethylhydrazino)propionate (146 g, 1 mol) in water (290 mL) and heat at 90-100 °C under an inert atmosphere until the starting ester Complete conversion to the corresponding acid (monitored by HPLC). Methanol (150 mL) was added to the reaction mixture, followed by dimethyl carbonate (843 mL, 10 mol). The reaction mixture was heated in the reactor at 90 °C until completion of the reaction (monitored by HPLC). Methanol, dimethyl carbonate and water were removed by distillation under reduced pressure. The distillation residue was dissolved in hot isopropanol (500ml) and evaporated again. The obtained 3-(2,2,2-trimethylhydrazine)propionate dihydrate was dried under reduced pressure. Yield 172 g (94.4%).

Embodiment 2

[0021] Preparation of 3-(2,2,2-trimethylhydrazine)propionate dihydrate

[0022] Dissolve methyl 3-(2,2-dimethylhydrazino)propionate (146 g, 1 mol) in water (270 mL), then add methanol (170 mL) and dimethyl carbonate (843 mL, 10 mol) to the solution ). The reaction mixture was heated in the reactor at 95°C until completion of the reaction (monitored by HPLC). Methanol, dimethyl carbonate and water were removed by distillation under reduced pressure. The distillation residue was dissolved in hot isopropanol (500ml) and evaporated again. The obtained 3-(2,2,2-trimethylhydrazine)propionate dihydrate was dried under reduced pressure. Yield 171 g (93.9%).

Embodiment 3

[0024] Preparation of 3-(2,2,2-trimethylhydrazine)propionate dihydrate

[0025] 3-(2,2-Dimethylhydrazino)propionic acid (132 g, 1 mol) was dissolved in water (180 mL), then methanol (170 mL) and dimethyl carbonate (843 mL, 10 mol) were added to the reaction mixture ). The reaction mixture was heated in the reactor at 95°C until completion of the reaction (monitored by HPLC). Methanol, dimethyl carbonate and water were removed by distillation under reduced pressure. The distillation residue was dissolved in hot isopropanol (500ml) and evaporated again. The obtained 3-(2,2,2-trimethylhydrazine)propionate dihydrate was dried under reduced pressure. Yield 175 g (96.0%).

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Abstract

The present invention relates to one-pot process for preparing 3-(2,2,2-trimethylhydrazinium)propionate dihydrate from 3-(2,2-dimethylhydrazino)propionate esters.

Description

technical field [0001] The present invention relates to 3-(2,2-dimethylhydrazino) propionate (wherein, R represents CH) by general formula (I) 3 、C 2 h 5 、C 3 h 7 , i-C 3 h 7 、C 4 h 9 , i-C 4 h 9 and C 6 h 5 CH 2 ) and a one-pot method for the preparation of 3-(2,2,2-trimethylhydrazine)propionate dihydrate (International Nonproprietary Name—"Meldonium") from the corresponding acid (R for H). [0002] Background technique [0003] 3-(2,2,2-Trimethylhydrazine) propionate dihydrate with the International Nonproprietary Name Meldonium is known for its cardioprotective effects. Various methods are known for the preparation of 3-(2,2,2-trimethylhydrazine)propionate dihydrate. [0004] Typically, the process involves reaction of 1,1-dimethylhydrazine with acrylate to form 3-(2,2-dimethylhydrazino)propionate, further alkylation with methyl halide or dimethyl sulfate The appropriate methyl 3-(2,2,2-trimethylhydrazine)propionate halide or methyl sulfate is produced, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C241/02C07C243/40
CPCC07C243/40
Inventor 伊瓦尔斯·卡尔温斯普戈威克斯·奥斯瓦尔迪斯亚力山德拉斯·切尔诺不罗维吉斯阿格尼娅·依维娜安东斯·列别杰夫斯
Owner GRINDEKS
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