反应详情

温度

22.5 °C

Under N2, bis(2-chlorophenyl)methanol (70 g, 0.28 mol) was added in 4 portions at 20 to 25° C. to HBr (97 ml) in acetic acid (33% by weight). The mixture was stirred at 20 to 25° C. and the reaction was followed by HPLC. After complete reaction (60 to 90 min), the mixture was cooled to 0 to 10° C. and water (700 ml) was added over 30 min. The suspension was stirred at 0 to 10° C. for a further 30 min. The product was isolated by filtration and washed with water (4×140 ml). The product was dried under vacuum at 25° C. to constant weight. Yield: 82.6 g (95%). Assay (HPLC): 100% pure vs. standard

1. customAfter complete reaction (60 to 90 min)
2. temperaturethe mixture was cooled to 0 to 10° C.
3. stirringThe suspension was stirred at 0 to 10° C. for a further 30 min
4. customThe product was isolated by filtration
5. washwashed with water (4×140 ml)
6. customThe product was dried under vacuum at 25° C. to constant weight