반응 #60807

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Sodium thiomethoxide

4-chlorothieno[3,2-d]pyrimidine

water

→

title compound

수율 69.0%

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

수율 69.0%

용매

DMF

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후처리

1. 1
   추출extracted into EtOAc
2. 2
   세척washed with water
3. 3
   건조dried (MgSO4)
4. 4
   기타the solvent removed
5. 5
   기타Purification by flash chromatography on silica eluting with DCM:EtOAc (4:1)

실험 절차

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%);

출처