反应详情

温度

0 °C

1-(2-Amino-3-chloro-4-methoxyphenyl)ethanone (prepared according to Raboisson, P. J.-M. B., et al., WO2007014926, p 78; 70.7 g, 354 mmol) was stirred in 48% aq. HBr (500 mL) at 110° C. for 72 h. After the mixture was cooled to 0° C. with stirring, the solids were filtered and washed with water. The resulting solids were triturated with a saturated NaHCO3 solution (−350 mL), filtered, washed with water, and dried under vacuum to give 40 g (61% yield) of 1-(2-amino-3-chloro-4-hydroxyphenyl)ethanone as a dark brown solid.

1. filtrationthe solids were filtered
2. washwashed with water
3. customThe resulting solids were triturated with a saturated NaHCO3 solution (−350 mL)
4. filtrationfiltered
5. washwashed with water
6. customdried under vacuum