反应详情

Crude 5-(tert-butoxycarbonylaminomethyl)-3-cyclopropylisoxazole (Method 3) (37.4 g, 0.157 mol) and 3M hydrochloric acid (80 ml) in methanol (100 ml) was heated at 50° C. for 2 hours. The methanol was removed by evaporation and aqueous residue washed with DCM. The aqueous layer was adjusted to pH 12 by careful addition of 40% aqueous sodium hydroxide solution and then extracted with DCM (×4). The extracts were combined, washed with brine, then dried (Na2SO4) and the volatiles removed by evaporation to give the title compound (11.5 g, 53%) as oil.

1. customThe methanol was removed by evaporation and aqueous residue
2. washwashed with DCM
3. additionThe aqueous layer was adjusted to pH 12 by careful addition of 40% aqueous sodium hydroxide solution
4. extractionextracted with DCM (×4)
5. washwashed with brine
6. dry with materialdried (Na2SO4)
7. customthe volatiles removed by evaporation