Dichloromethane → 4-((3-Bromothiophen-2-yl)methyl)morpholine
反応式
[Br:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[CH:7]=O.[NH:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1.C(Cl)Cl.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>CCOC(C)=O>[Br:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[CH2:7][N:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1参加物
6
実験手順
To a solution of 3-bromothiophene-2-carbaldehyde (500 mg, 2.62 mmol) and morpholine (0.68 mL, 7.85 mmol) and CH2Cl2 (10 mL) was added sodium triacetoxyborohydride (1.11 g, 5.24 mmol). The mixture was stirred at room temperature overnight. The resulting mixture was diluted with EtOAc (100 mL) and the organic layer was washed with brine then dried (Na2SO4), filtered and concentrated. The residue was purified by column chromatography (silica, 0-5% MeOH in CH2Cl2) to afford the sub-title compound (580 mg, 84%).
後処理
- washthe organic layer was washed with brine
- dry with materialthen dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by column chromatography (silica, 0-5% MeOH in CH2Cl2)
出典と根拠
- ORDレコード
- ord-5381ad921d964fcfabc70626713bb363
- 出典データセット
- uspto-grants-2012_12
- 特許番号
- US08324264B1
反応ノート
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