Sodium borohydride → 2,2-Difluoro-2-phenylethanol
反応式
C([O:3][C:4](=O)[C:5]([F:13])([F:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)C.[BH4-].[Na+]>C(O)C>[F:12][C:5]([F:13])([C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)[CH2:4][OH:3]参加物
4
実験手順
A stirred mixture of 2.2 g of difluoro-2-phenyl acetic acid ethyl ester (W. J. Middleton, E. M. Bingham, J. Org. Chem., 45, 2883-2887 (1980)), and 0.6 g of sodium borohydride in 75 mL of ethanol was kept at room temperature overnight, concentrated to near dryness under reduced pressure carefully acidified with 20 mL of 5% HCl and extracted into 3×50 mL of dichloromethane. The combined extracts were dried over magnesium sulfate and concentrated under reduced pressure. Drying under vacuum gave 1.7 g of product as an oil: 1H NMR (400 MHz, CDCl3) 7.5 (m, 5H), 4.0 (t, 2H).
後処理
- concentrationconcentrated
- extractionextracted into 3×50 mL of dichloromethane
- dry with materialThe combined extracts were dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customDrying under vacuum
出典と根拠
- ORDレコード
- ord-9e6fbc5b68eb4c49afe95970aca491c6
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07452893B2
反応ノート
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