Isoamyl Nitrite → 3-Methyl-4-(trifluoromethyl)benzonitrile
反応式
N[C:2]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[C:7]([CH3:14])=[CH:6][C:3]=1[C:4]#[N:5].N(OCCC(C)C)=O>C1COCC1.CC(OC)(C)C>[CH3:14][C:7]1[CH:6]=[C:3]([CH:2]=[CH:9][C:8]=1[C:10]([F:11])([F:12])[F:13])[C:4]#[N:5]参加物
5
反応条件
- 温度
- 23 °C
実験手順
To a solution of 2-amino-5-methyl-4-trifluoromethyl-benzonitrile from step 4 (23.34 g, 117 mmol) in dry THF (350 mL) was added isoamyl nitrite (34.3 mL, 257 mmol), and the mixture was refluxed for 20 h. Additional isoamyl nitrite (16.6 mL, 129 mmol) was added and the mixture was refluxed for further 20 h. The mixture was cooled to 23° C. and diluted with TBME, the organic layer was washed with 1 N HCl, sat. NaHCO3-sol. and brine, dried over Na2SO4.
後処理
- temperaturethe mixture was refluxed for 20 h
- temperaturethe mixture was refluxed for further 20 h
- washthe organic layer was washed with 1 N HCl, sat. NaHCO3-sol
- dry with materialand brine, dried over Na2SO4
出典と根拠
- ORDレコード
- ord-46697044b81f4e88bf8c20af30d17f25
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07446113B2
反応ノート
読み込み中…