Thionyl Chloride → 7-(Chloromethyl)-5,6-difluoro-2,2-dimethyl-2,3-dihydrobenzofuran
반응식
[F:1][C:2]1[C:3]([F:15])=[C:4]([CH2:13]O)[C:5]2[O:9][C:8]([CH3:11])([CH3:10])[CH2:7][C:6]=2[CH:12]=1.O=S(Cl)[Cl:18]>ClCCl>[Cl:18][CH2:13][C:4]1[C:5]2[O:9][C:8]([CH3:11])([CH3:10])[CH2:7][C:6]=2[CH:12]=[C:2]([F:1])[C:3]=1[F:15]참가 물질
4
실험 절차
To a solution of (5,6-difluoro-2,2-dimethyl-3H-benzofuran-7-yl)methanol (736) (0.18 g, 0.84 mmol) in anhydrous dichloromethane (5 mL) was added SOCl2 dropwise at 0° C. The mixture was stirred at room temperature for 2 h. The solvent was removed in vacuo, and the residue was dissolved in EtOAc (100 mL). The solution was washed with water (30 mL), dried over anhydrous sodium sulfate, and evaporated in vacuo to give a solid 7-(chloromethyl)-5,6-difluoro-2,2-dimethyl-2,3-dihydrobenzofuran (737) (0.194 g, 99%).
후처리
- customThe solvent was removed in vacuo
- dissolutionthe residue was dissolved in EtOAc (100 mL)
- washThe solution was washed with water (30 mL)
- dry with materialdried over anhydrous sodium sulfate
- customevaporated in vacuo
출처 및 근거
- ORD 기록
- ord-6d1ab824835b40cebe04787b4b1a266a
- 출처 데이터셋
- uspto-grants-2013_12
- 특허 번호
- US08598374B2
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