反应详情

温度

-20 °C

1.57 ml of phosgene (20% solution in toluene, 2.96 mmol) were initially charged in 5 ml of dichloroethane and cooled to −20° C., then a mixture of 8-azaspiro-[4,5]decane (750 mg, 2.96 mmol) and triethylamine (1.28 ml, 9.2 mmol, 3.1 eq.) was added slowly. After 30 min, the mixture was allowed to come to RT; after 1 h, according to LC-MS, a little starting material was still present but also three new peaks. Subsequently, the mixture was added to 2 N aqueous HCl, the aqueous phase was extracted with dichloromethane, and the organic phase was washed with saturated NaHCO3 solution and dried over sodium sulfate; subsequently, the mixture was concentrated by rotary evaporation under reduced pressure. Crude yield: 592 mg

1. additionwas added slowly
2. customto come to RT
3. waitafter 1 h
4. extractionthe aqueous phase was extracted with dichloromethane
5. washthe organic phase was washed with saturated NaHCO3 solution
6. dry with materialdried over sodium sulfate
7. concentrationsubsequently, the mixture was concentrated by rotary evaporation under reduced pressure