Reaktion #307271

Reaktionsgleichung

(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

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis heated
2. 2
   Temperaturto reflux for 4 hours
3. 3
   EinengenThe reaction mixture is then concentrated
4. 4
   Sonstigetriturated with water (10 mL)
5. 5
   FiltrationAfter filtration
6. 6
   Waschenthe undissolved solid is further washed with water
7. 7
   Sonstigeair-dried

Vorschrift

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.

Quelle