反应详情

2.10 g (5.4 mmol) of 4-(3-cyanomethoxy-5-methoxy-benzoylamino)-piperidine-1-carboxylic acid tert-butyl ester (example 245) and 0.15 g (1.1 mmol) of potassium carbonate were suspended under argon in 10 mL of DMSO at rt; while stirring, 0.93 mL (1.05 g=2.0 eq.) of hydrogen peroxide solution (35% in water) was added below 25° C. and stirring continued at ambient temperature for 24 hours. Then, the reaction mixture was poured into crashed ice and extracted three times with MeCl2 /2-propanol (4:1); the organic phases were evaporated i.V. to yield 2.26 g of the crude title compound as colorless solid. MS: 408.1 (MH+).

1. stirringstirring
2. additionThen, the reaction mixture was poured
3. extractionextracted three times with MeCl2 /2-propanol (4:1)
4. customthe organic phases were evaporated i.V