反应详情

温度

90 °C

To a solution of tert-butyl 4-(3-((3SR,5SR)-3-(2-chloro-4-fluorophenyl)-5-hydroxy-2-oxopiperidin-1-yl)thioureido)piperidine-1-carboxylate (1.2 g, 2.4 mmol) in DMF (5 mL) was added iodomethane (0.2 mL, 3.6 mmol) and the reaction heated to 90° C. for 15 minutes. The reaction was evaporated to dryness, redissolved in ethyl acetate, washed with saturated sodium hydrogen carbonate, water, brine, dried with sodium sulfate and the solvent was evaporated in vacuo. The title compound, a mixture of geometrical isomers, was used crude in the next step (1.2 g, 99%).

1. customThe reaction was evaporated to dryness
2. dissolutionredissolved in ethyl acetate
3. washwashed with saturated sodium hydrogen carbonate, water, brine
4. dry with materialdried with sodium sulfate
5. customthe solvent was evaporated in vacuo
6. additionThe title compound, a mixture of geometrical isomers