반응 #73555

반응 방정식

(2,2-difluoro-benzo[1,3]dioxol-5-yl)-methanol

dichloromethane

→

5-chloromethyl-2,2-difluoro-benzo[1,3]dioxole

반응 조건

후처리

1. 1
   기타evaporated to dryness
2. 2
   기타The residue was partitioned between an aqueous solution of saturated sodium bicarbonate (100 mL) and dichloromethane (100 mL)
3. 3
   추출The separated aqueous layer was extracted with dichloromethane (150 mL)
4. 4
   건조the combined organic layers were dried over sodium sulfate
5. 5
   여과filtrated
6. 6
   기타evaporated to dryness

실험 절차

5-Chloromethyl-2,2-difluoro-benzo[1,3]dioxole Thionyl chloride (45 g, 38 mmol) was slowly added to a solution of (2,2-difluoro-benzo[1,3]dioxol-5-yl)-methanol (7.2 g, 38 mmol) in dichloromethane (200 mL) at 0° C. The resulting mixture was stirred overnight at room temperature and then evaporated to dryness. The residue was partitioned between an aqueous solution of saturated sodium bicarbonate (100 mL) and dichloromethane (100 mL). The separated aqueous layer was extracted with dichloromethane (150 mL) and the combined organic layers were dried over sodium sulfate, filtrated, and evaporated to dryness to give crude 5-chloromethyl-2,2-difluoro-benzo[1,3]dioxole (4.4 g) which was used directly in the next step.

출처