반응 #9866

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4-chloro-2-methylsulfanyl-thieno[2,3-d]pyrimidine

OXONE

tetrahydrofuran

→

title compound

4—Chloro-2-methanesulfonyl-thieno[2,3-d]pyrimidine

용매

water

ethyl acetate

water

반응 조건

후처리

1. 1
   온도The resulting mixture was gradually warmed from 0° C. to room temperature overnight
2. 2
   기타the layers were separated
3. 3
   추출The aqueous layer was extracted with ethyl acetate (1×300 mL)
4. 4
   세척washed with brine (2×300 mL)
5. 5
   건조dried over magnesium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated

실험 절차

To a solution of 4-chloro-2-methylsulfanyl-thieno[2,3-d]pyrimidine (10 g, 46.15 mmol) in tetrahydrofuran (350 mL) at 0° C. was added a solution of OXONE (59.6 g, 2.1 eq) in water (300 mL) dropwise with stirring. The resulting mixture was gradually warmed from 0° C. to room temperature overnight. The reaction mixture was diluted with ethyl acetate (1000 mL) and water (300 mL), and the layers were separated. The aqueous layer was extracted with ethyl acetate (1×300 mL). Organic layers were combined, washed with brine (2×300 mL), dried over magnesium sulfate, filtered and concentrated to give 10.7 g of the title compound as a tan powder (M+H)+=249.

출처