2-Methylbenzamide → Benzenecarboximidic acid, 2-methyl-, ethyl ester
反応式
[C:1]1([CH3:10])[C:2]([C:7]([NH2:9])=[O:8])=[CH:3][CH:4]=[CH:5][CH:6]=1.F[B-](F)(F)F.[CH2:16]([O+](CC)CC)[CH3:17]>ClCCl>[CH3:10][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7](=[NH:9])[O:8][CH2:16][CH3:17]参加物
4
実験手順
To a solution of o-toluamide (13.5 g, 0.100 mol) in dichloromethane (150 mL) was added a solution (1.0 M, 106 mL, 0.106 mol) of triethyloxonium tetrafluoroborate in dichloromethane. The resulting mixture was stirred at room temperature for 14 h. Two-thirds of dichloromethane was evaporated under reduced pressure. After addition of ether (400 mL) to the concentrate, the mixture was stirred for 3 h under ice-cooling. Precipitates were collected by filtration, washed with ether, and dried in vacuo to give 21.7 g (86%) of ethyl 2-methylbenzimidate hydrotetrafluoroborate as a colorless solid.
後処理
- customTwo-thirds of dichloromethane was evaporated under reduced pressure
- additionAfter addition of ether (400 mL) to the concentrate
- stirringthe mixture was stirred for 3 h under ice-
- temperaturecooling
- customPrecipitates
- filtrationwere collected by filtration
- washwashed with ether
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-53d02a2dd54f4931b742aa5ac204913f
- 出典データセット
- uspto-grants-1999_09
- 特許番号
- US05948785
反応ノート
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