反応 #60807

反応方程式

Sodium thiomethoxide

4-chlorothieno[3,2-d]pyrimidine

water

→

title compound

収率 69.0%

4-(Methylthio)thieno[3,2-d]pyrimidine

収率 69.0%

溶媒

DMF

反応条件

後処理

1. 1
   抽出extracted into EtOAc
2. 2
   洗浄washed with water
3. 3
   乾燥dried (MgSO4)
4. 4
   その他the solvent removed
5. 5
   その他Purification by flash chromatography on silica eluting with DCM:EtOAc (4:1)

実験手順

Sodium thiomethoxide (9.1 g) was added to a solution of 4-chlorothieno[3,2-d]pyrimidine (WO9849899, example 3A; WO9924440, example 1C) (17.0 g) in DMF (100 mL). After stirring for 90 minutes the mixture was poured into water (400 mL), extracted into EtOAc, washed with water, dried (MgSO4), and the solvent removed. Purification by flash chromatography on silica eluting with DCM:EtOAc (4:1) gave the title compound as a pale yellow solid (16.5 g, 69%);

出典