Triethylamine → HCID 178426651、化合物
反応式
[Br:1][C:2]1[C:9]([CH3:10])=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[CH3:11].Cl.[NH2:13][OH:14].C(N(CC)CC)C>C(O)C>[Br:1][C:2]1[C:3]([CH3:11])=[CH:4][C:5]([C:6]([NH:13][OH:14])=[NH:7])=[CH:8][C:9]=1[CH3:10]参加物
5
実験手順
A mixture of 4-bromo-3,5-dimethyl-benzonitrile (1.50 g), hydroxylamine hydrochloride (0.90 g), triethylamine (1.8 mL) and ethanol (30 mL) is stirred at reflux temperature for 4 h. After cooling to room temperature, the mixture is concentrated, the residue is taken up in water, and the resulting mixture is extracted with ethyl acetate. The combined extract is washed with brine, dried (Na2SO4), and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 7:3→3:7) to give the title compound. LC (method 11): tR=0.73 min; Mass spectrum (ESI+): m/z=243/245 (Br) [M+H]+.
後処理
- temperatureat reflux temperature for 4 h
- concentrationthe mixture is concentrated
- extractionthe resulting mixture is extracted with ethyl acetate
- extractionThe combined extract
- washis washed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 7:3→3:7)
出典と根拠
- ORDレコード
- ord-fe2b26db05e3496a8c9f94e8def1af03
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08642585B2
反応ノート
読み込み中…