Pivaloyl chloride → 1-Benzothiophen-6-YL 2,2-dimethylpropanoate
反応式
[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=2参加物
4
実験手順
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%).
後処理
- 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
出典と根拠
- ORDレコード
- ord-b9162a7dbdd346cf923519bd1c60a8fd
- 出典データセット
- uspto-grants-2009_09
- 特許番号
- US07585977B2
反応ノート
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