Thionyl Chloride → 7-(Chloromethyl)-5,6-difluoro-2,2-dimethyl-2,3-dihydrobenzofuran
反応式
[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]参加物
4
実験手順
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%).
後処理
- 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
出典と根拠
- ORDレコード
- ord-1e2ddd3b929a45fe8369cc6d87c49c87
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08309600B2
反応ノート
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