Sodium borohydride → HCID 57443976、化合物
反応式
[C:1]([C:4]1[CH:17]=[CH:16][C:7]2[CH:8]=[C:9]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[S:10][C:6]=2[CH:5]=1)(=[O:3])[CH3:2].[BH4-].[Na+]>C1COCC1.CCO>[OH:3][CH:1]([C:4]1[CH:17]=[CH:16][C:7]2[CH:8]=[C:9]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[S:10][C:6]=2[CH:5]=1)[CH3:2]参加物
4
実験手順
To a cooled (0° C.) solution of ethyl 6-acetyl-1-benzothiophene-2-carboxylate (2.0 g, 8.06 mmol) in THF/EtOH (20/20 mL) was added sodium borohydride (308 mg, 8.14 mmol) portionwise. After 2 h, the reaction was quenched with sat. NH4Cl. The resulting mixture diluted with EtOAc (40 mL), washed with water and brine. The organic layer was dried over Na2SO4, filtered and concentrated. The resultant residue (2.1 g) was used without further purification. MS (EI): cal'd 251 (MH+), exp 251 (MH+).
後処理
- customthe reaction was quenched with sat. NH4Cl
- additionThe resulting mixture diluted with EtOAc (40 mL)
- washwashed with water and brine
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe resultant residue (2.1 g) was used without further purification
出典と根拠
- ORDレコード
- ord-12774d699f8349848baf8fe73c7b78c3
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07772238B2
反応ノート
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