Chlorosuccinimide → N-Hydroxy-2-(trifluoromethyl)benzene-1-carboximidoyl chloride
反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[CH:5]=[N:6][OH:7].[Cl:14]N1C(=O)CCC1=O>>[OH:7][N:6]=[C:5]([Cl:14])[C:4]1[CH:8]=[CH:9][CH:10]=[CH:11][C:3]=1[C:2]([F:12])([F:13])[F:1]参加物
3
実験手順
2-(trifluoromethyl)benzaldehydeoxime (30.0 g, 158.60 mmol) was dissolved in dimethylformimide (300 mL), and added with N-chlorosuccinimide (23.31 g, 174.46 mmol), followed by stirring for 15 hours. After the reaction was completed, the resultant solution was vacuum evaporated, added with ethylacetate (1,500 mL), washed with saturated sodium chloride aqueous solution (1,000 mL) and purified water (1,000 mL), respectively, dried with anhydrous sodium sulfate, and vacuum-evaporated to provide a pale yellow solid required compound (32.81 g, 146.70 mmol, 93%).
後処理
- customevaporated
- additionadded with ethylacetate (1,500 mL)
- washwashed with saturated sodium chloride aqueous solution (1,000 mL)
- custompurified water (1,000 mL)
- dry with materialrespectively, dried with anhydrous sodium sulfate
- customvacuum-evaporated
出典と根拠
- ORDレコード
- ord-b510498aac614bb1911441cdc1175ce2
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09132126B2
反応ノート
読み込み中…