Pivaloyl chloride → 1-Benzothiophen-6-YL 2,2-dimethylpropanoate
반응식
[S:1]1[CH:5]=[CH:4][C:3]2[CH:6]=[CH:7][C:8]([OH:10])=[CH:9][C:2]1=2.[CH3:11][C:12]([CH3:17])([CH3:16])[C:13](Cl)=[O:14]>N1C=CC=CC=1>[S:1]1[CH:5]=[CH:4][C:3]2[CH:6]=[CH:7][C:8]([O:10][C:13](=[O:14])[C:12]([CH3:17])([CH3:16])[CH3:11])=[CH:9][C:2]1=2참가 물질
4
실험 절차
Dissolve benzo[b]thiophen-6-ol (10 g, 67 mmol) in pyridine (300 mL). Add 2,2-dimethyl-propionyl chloride (38 mL, 308 mmol) dropwise, and stir at room temperature for 8 hours. Concentrate in vacuo to ¼ Volume, partition between ethyl acetate (250 mL) and water (250 mL). Separate layers, wash organic layer with water (250 mL) and brine (200 mL). Dry with magnesium sulfate, filter, and concentrate in vacuo to give 15 g of 2,2-dimethyl-propionic acid benzo[b]thiophen-6-yl ester (98%).
후처리
- concentrationConcentrate in vacuo
- custompartition between ethyl acetate (250 mL) and water (250 mL)
- washSeparate layers, wash organic layer with water (250 mL) and brine (200 mL)
- dry with materialDry with magnesium sulfate
- filtrationfilter
- concentrationconcentrate in vacuo
출처 및 근거
- ORD 기록
- ord-2b05473bda7542f7bc2e58ea90b282e1
- 출처 데이터셋
- uspto-grants-2008_07
- 특허 번호
- US07399867B2
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