反应详情

0.860 g (2.49 mmol) of tert-butyl 4-(5-(trifluoromethyl)(pyridin-2-ylamino)piperidine-1-carboxylate obtained in stage 6.1. is dissolved in 8.5 ml of dichloromethane. 1.91 ml of trifluoroacetic acid are added and the mixture is stirred at ambient temperature for 4 hours. The dichloromethane is evaporated and then the residue is coevaporated twice with 10 ml of 1,2-dichloroethane. The residue is taken up in a mixture of 50 ml of ethyl acetate, 10 ml of a 1N aqueous sodium hydroxide solution and 5 ml of a 33% aqueous ammonia solution. The organic phase is separated by settling. It is washed with 2 times 10 ml of water and then with 10 ml of a saturated aqueous sodium chloride solution. It is dried over sodium sulphate and evaporated to dryness to produce 0.572 g (2.33 mmol) of product in the form of an off-white solid.

1. customThe dichloromethane is evaporated
2. additionThe residue is taken up in a mixture of 50 ml of ethyl acetate, 10 ml of a 1N aqueous sodium hydroxide solution and 5 ml of a 33% aqueous ammonia solution
3. customThe organic phase is separated
4. washIt is washed with 2 times 10 ml of water
5. dry with materialIt is dried over sodium sulphate
6. customevaporated to dryness