반응 #324579

반응 방정식

2-amino-4-chloro-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

benzo[1,3]dioxol-5-yl-acetonitrile

sodium hydride

→

2-Amino-4-(benzo[1,3]dioxol-5-yl-cyano-methyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

용매

DMF

brine

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate
2. 2
   세척The combined organic portions were washed with brine and water
3. 3
   건조dried with sodium sulphate
4. 4
   여과After filtration and evaporation of the solvent
5. 5
   기타brown solids were obtained which
6. 6
   기타were purified either by preparative TLC or preparative HPLC

실험 절차

To a solution of 2-amino-4-chloro-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (1 equiv.) and benzo[1,3]dioxol-5-yl-acetonitrile (1 mole eq.) in DMF at room temperature, sodium hydride (1.1 mole eq., 60% in mineral oil) was added. The mixture was stirred at this temperature overnight under argon. After that, it was diluted with brine and extracted with ethyl acetate. The combined organic portions were washed with brine and water and dried with sodium sulphate. After filtration and evaporation of the solvent, brown solids were obtained which were purified either by preparative TLC or preparative HPLC.

출처