反应详情

A suspension of 4-bromo-3-(trifluoromethyl)aniline HCl salt (36.8 g, 133 mmol) in toluene (278 mL) was treated with trichloromethyl chloroformate dropwise and the resulting mixture was heated at the reflux temp. for 18 h. The resulting mixture was concentrated under reduced pressure. The residue was treated with toluene (500 mL), then concentrated under reduced pressure. The residue was treated with CH2Cl2 (500 mL), then concentrated under reduced pressure. The CH2Cl2 treatment/concentration protocol was repeated and resulting amber oil was stored at −20° C. for 16 h, to afford 4-bromo-3-(trifluoromethyl)phenyl isocyanate as a tan solid (35.1 g, 86%): GC-MS m/z 265 (M+).

1. temperaturethe resulting mixture was heated at the reflux temp
2. concentrationThe resulting mixture was concentrated under reduced pressure
3. additionThe residue was treated with toluene (500 mL)
4. concentrationconcentrated under reduced pressure
5. additionThe residue was treated with CH2Cl2 (500 mL)
6. concentrationconcentrated under reduced pressure
7. concentrationThe CH2Cl2 treatment/concentration protocol
8. customresulting amber oil
9. waitwas stored at −20° C. for 16 h