반응 #47847

반응 방정식

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

THF

OXONE

→

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

용매

EtOAc

water

water

반응 조건

후처리

1. 1
   workup.STIRRINGThe resulting mixture was stirred at RT overnight
2. 2
   기타Separated the layers
3. 3
   추출the aqueous layer was extracted with EtOAc (3×300 mL)
4. 4
   세척washed with brine (2×300 mL)
5. 5
   건조dried over MgSO4
6. 6
   여과filtered
7. 7
   농축concentrated
8. 8
   기타to give (33 g)

실험 절차

To 1 L round-bottom flask was added 4-chloro-2-(methylthio)thieno[2,3-d]pyrimidine (35.0 g, 162 mmol), THF (300 mL). The solution was stirred at 0° C. and treated dropwise with a solution of OXONE (209 g, 339 mmol) in water (350 mL). The resulting mixture was stirred at RT overnight. The reaction mixture was diluted with EtOAc (500 mL) and water (300 mL). Separated the layers, the aqueous layer was extracted with EtOAc (3×300 mL). Organic layers were combined, washed with brine (2×300 mL), dried over MgSO4, filtered and concentrated to give (33 g). MS (ES+): 249 (M+H)+.

출처