Sodium borohydride → HCID 69353261、化合物
反応式
[BH4-].[Na+].[Br:3][C:4]1[CH:5]=[C:6]([N+:14]([O-:16])=[O:15])[C:7]([O:12][CH3:13])=[C:8]([CH:11]=1)[CH:9]=[O:10]>CO.O1CCCC1>[Br:3][C:4]1[CH:5]=[C:6]([N+:14]([O-:16])=[O:15])[C:7]([O:12][CH3:13])=[C:8]([CH:11]=1)[CH2:9][OH:10]参加物
5
実験手順
Sodium borohydride (4 g) was added in portions to a stirring solution of crude 5-bromo-2-methoxy-3-nitrobenzaldehyde (20.5 g) in methanol (350 mL) and tetrahydrofuran (150 mL) at 0° C. After 1 h, the methanol was removed in vacuo. The residue was treated with cold water (150 mL) and extracted with diethyl ether (2×150 mL). The combined organic layer was evaporated in vacuo to give a crude oil. Silica gel chromatography eluting with ethyl acetate in petroleum ether (10–40%) gave the title compound (17 g) as a solid.
後処理
- customthe methanol was removed in vacuo
- additionThe residue was treated with cold water (150 mL)
- extractionextracted with diethyl ether (2×150 mL)
- customThe combined organic layer was evaporated in vacuo
- customto give a crude oil
- washSilica gel chromatography eluting with ethyl acetate in petroleum ether (10–40%)
出典と根拠
- ORDレコード
- ord-1f72f1a800ac48aeb6e9e41e2e9b490f
- 出典データセット
- uspto-grants-2007_05
- 特許番号
- US07214674B2
反応ノート
読み込み中…