反应详情

To a solution of 1-tert-butoxycarbonylaminocyclopropanecarboxylic acid (2.32 g, 11.5 mmol) in CH2Cl2 (25 mL) at 0° C. was added N,O-dimethylhydroxylamine hydrochloride (1.24 g, 12.7 mmol), triethylamine (2.57 g, 3.54 mL, 25.4 mmol), and HATU (4.82 g, 12.7 mmol). The reaction mixture was stirred at room temperature for 4 h. The reaction mixture was concentrated under reduced pressure and then partitioned between Et2O and water. The water layer was extracted with Et2O. The combined organic layer was washed with brine, dried (Na2SO4), and concentrated under reduced pressure to yield [1-(methoxy-methyl-carbamoyl)-cyclopropyl]carbamic acid tert-butyl ester which was used in the next step without further purification.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. custompartitioned between Et2O and water
3. extractionThe water layer was extracted with Et2O
4. washThe combined organic layer was washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated under reduced pressure