反応 #307271

反応方程式

(6-hydrazino-pyrimidin-4-yl)-methyl-carbamic acid tert-butyl ester

2-cyano-3-ethoxy-acrylic acid ethyl ester

→

5-amino-1-[6-(tert-butoxycarbonyl-methyl-amino)-pyrimidin-4-yl]-1H-pyrazole-4-carboxylic acid ethyl ester

溶媒

ethanol

反応条件

後処理

1. 1
   温度is heated
2. 2
   温度to reflux for 4 hours
3. 3
   濃縮The reaction mixture is then concentrated
4. 4
   その他triturated with water (10 mL)
5. 5
   ろ過After filtration
6. 6
   洗浄the undissolved solid is further washed with water
7. 7
   その他air-dried

実験手順

A mixture of (6-hydrazino-pyrimidin-4-yl)-methyl-carbamic acid tert-butyl ester (4.0 g, 16.7 mmol), 2-cyano-3-ethoxy-acrylic acid ethyl ester (3.02 g, 17.5 mmol) and ethanol (25 mL) is heated to reflux for 4 hours. The reaction mixture is then concentrated and triturated with water (10 mL). White precipitate forms. After filtration, the undissolved solid is further washed with water, then air-dried to give 5-amino-1-[6-(tert-butoxycarbonyl-methyl-amino)-pyrimidin-4-yl]-1H-pyrazole-4-carboxylic acid ethyl ester as white powder.

出典