Sodium borohydride → HCID 67252978、化合物
反応式
[CH3:1][C:2]1[CH:9]=[CH:8][C:7]([N:10]2[N:14]=[CH:13][CH:12]=[N:11]2)=[CH:6][C:3]=1[CH:4]=[O:5].[BH4-].[Na+]>CO>[CH3:1][C:2]1[CH:9]=[CH:8][C:7]([N:10]2[N:14]=[CH:13][CH:12]=[N:11]2)=[CH:6][C:3]=1[CH2:4][OH:5]参加物
4
実験手順
To a stirred solution of 2-methyl-5-(2H-1,2,3-triazol-2-yl)benzaldehyde (140 mg, 0.75 mmol) in methanol (10 mL), NaBH4 (42 mg, 1.1 mmol) was added at 10° C. and stirred for 10 min. Then the mixture was allowed to warm to rt and stirred for 1 h. The mixture was quenched with saturated aqueous NH4Cl solution (0.3 mL) and filtered over hyflow. The filtrate was dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The crude product was purified flash column chromatography (eluent: 30% ethyl acetate in hexane) to yield the title compound (100 mg, 71%). [TLC Rf=0.18 (ethyl acetate/hexane 30:70)].
後処理
- stirringstirred for 1 h
- customThe mixture was quenched with saturated aqueous NH4Cl solution (0.3 mL)
- filtrationfiltered over hyflow
- dry with materialThe filtrate was dried over anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe crude product was purified flash column chromatography (eluent: 30% ethyl acetate in hexane)
出典と根拠
- ORDレコード
- ord-d8c95a0dbc484268999aa328ae7e3d70
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08530648B2
反応ノート
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