反应详情

A mixture of 1.4 g (5 mmol) 4-acetoxy-1-benzyl-piperidine-4-carboxylic acid 0.49 mL (5.8 mmol) oxalylchloride, cat. amount DMF and 2.1 mL (15 mmol) NEt3 in DCM at 0° C. was stirred for 1 h. The mixture was concentrated and to 0.79 g (2.42 mmol) of the acid chloride and 2.1 mL (12.1 mmol) DIPEA in 25 mL DCM was added 0.554 g (2.9 mmol) methyl-(4-trifluoromethoxy-phenyl)-amine. The mixture was stirred for 15 h at room temperature. KHSO4 (1N) was added and the mixture was extracted with DCM. The combined organic extracts were dried with MgSO4 and evaporated. 0.782 g (72%) of the title compounds as obtained. MS (m/e): 451.3 [(M+H)+].

1. customat 0° C.
2. stirringThe mixture was stirred for 15 h at room temperature
3. extractionthe mixture was extracted with DCM
4. dry with materialThe combined organic extracts were dried with MgSO4
5. customevaporated