Oxalyl chloride → 2-Fluorobenzoyl isocyanate
反応式
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].C(Cl)(=O)[C:12](Cl)=[O:13]>ClCCCl>[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([N:6]=[C:12]=[O:13])=[O:5]参加物
4
反応条件
- 温度
- 100 °C
実験手順
0.47 g (3.0 mmol) of 2-fluorobenzamide and 0.40 g (3.2 mmol, 1.05 eq) of oxalyl chloride were added to 10 ml of 1,2-dichloroethane and then the mixture was stirred for 8 hours at 100° C. The reaction solution was cooled down to room temperature. The reaction solvent and excessive oxalyl chloride were removed by distillation under reduced pressure to obtain 2-fluorobenzoyl isocyanate in an oily state. 10 ml of fresh 1,2-dichloroethane and 0.95 g (3.0 mmol) of 2,4-dibromo-5-trifluoromethyl aniline were successively added thereto, reacted for 2 hours and filtered to obtain 1.11 g (Yield 77%) of the title compound as a solid.