Hydrochloric Acid → 2-(6-Chloropyridin-3-yl)ethan-1-ol
反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][C:9](O)=[O:10])=[CH:4][CH:3]=1.B.Cl.C(=O)(O)[O-].[Na+]>C1COCC1>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][CH2:9][OH:10])=[CH:4][CH:3]=1参加物
6
実験手順
To solid (6-chloro-pyridin-3-yl)-acetic acid (172 mg, 1 mmol) was added borane in THF (1M, 5 ml) and the reaction was stirred at room temperature. After 2 hours, the reaction was heated to 50 degC for 90 minutes. Aqueous hydrochloric acid (2N, 8 ml) was added to the reaction and it was allowed to cool to room temperature. After 10 minutes the reaction was basified with saturated aqueous sodium bicarbonate and extracted into ethyl acetate. The organic liquors were washed with water (×2) and brine, dried (MgSO4) and concentrated to furnish the crude product as a yellow oil (126 mg). This material was used as such in the coupling reaction. MS: [M+H]+158.
後処理
- temperaturethe reaction was heated to 50 degC for 90 minutes
- temperatureto cool to room temperature
- extractionextracted into ethyl acetate
- washThe organic liquors were washed with water (×2) and brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-a7af09d1d98e49b48ce8971dc0cc85f2
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08796244B2
反応ノート
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