Diisobutylaluminum hydride → 2-(6-Chloropyridin-2-yl)ethanol
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][C:9](OCC)=[O:10])[N:3]=1.CC(C[AlH]CC(C)C)C>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][CH2:9][OH:10])[N:3]=1参加物
4
実験手順
Ester 30-1 (1.34 g, 6.7 mmol) was dissolved in 10 mL CH2Cl2 at -78°, DIBAL (1M in CH2Cl2, 17 mL, 17 mmol) was added, the mixture was warmed to RT for 15 min before quenching in a mixture of 25 mL saturated aqueous Na-K tartrate and 100 mL EtOAc. This mixture was shaken vigorously. The phases were allowed to separate, and the organic layer was washed with brine, dried (MgSO4), concentrated and chromatographed (silica, 40% EtOAc/hexane), providing 30-2 as a yellow oil.
後処理
- custombefore quenching in a mixture of 25 mL saturated aqueous Na-K tartrate and 100 mL EtOAc
- customto separate
- washthe organic layer was washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customchromatographed (silica, 40% EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-4e935d9421444d4aae4963d5d0c851b2
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05929120
反応ノート
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