反应详情

To a stirred mixture of 17β-(3,4-methylenedioxybenzoyl)-estra-1,3,5(10)-triene-3-carboxaldehyde (0.041 g, 0,1 mmoles), tert-butyl alcohol (1.05 mL), 2-methyl-2-butene (4 mL of 2M solution in THF, 8 mmoles) at 0° C. was added a solution of NaClO2 (9 mg, 0.1 mmoles) and NaH2PO4. H2O (0.137 g, 0.1 mmoles) in H2O (0.4 ml) and stirred for 2 hours at ambient temperature. Acetic acid (glacial, 0.8 ml) and saturated NaCl solution (1.3 mL) were added to the reaction mixture which was extracted with EtOAc. The organic layer was washed with H2O, brine, dried (MgSO4), concentrated and azetroped with toluene. The resulting solid was triturated with CH3CN- acetone and filtered to give 0.02 g (47%) of the title compound as a white solid, mp 235°-237° C.

1. extractionwas extracted with EtOAc
2. washThe organic layer was washed with H2O, brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated and azetroped with toluene
5. customThe resulting solid was triturated with CH3CN- acetone
6. filtrationfiltered