반응 #324578

반응 방정식

2-Amino-4-(benzo[1,3]dioxole-5-carbonyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester

methyl magnesium bromide

→

desired compound

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

용매

THF

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타before being partitioned between 10% aqueous ammonium chloride solution and ethyl acetate
3. 3
   세척The organic layer was washed with brine
4. 4
   건조dried over magnesium sulphate
5. 5
   기타evaporated
6. 6
   기타to yield a crude product that
7. 7
   기타was purified by preparative TLC

실험 절차

2-Amino-4-(benzo[1,3]dioxole-5-carbonyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (example 312) (100 mg) was dissolved in anhydrous THF under a nitrogen atmosphere before methyl magnesium bromide (3.0M solution in diethyl ether, 5 equiv.) was added. The solution was stirred at 40° C. overnight before being partitioned between 10% aqueous ammonium chloride solution and ethyl acetate. The organic layer was washed with brine, dried over magnesium sulphate and evaporated to yield a crude product that was purified by preparative TLC to give the desired compound as a yellow powder.

출처