反应详情

A mixture of 1-acetyl-5-bromo-2-methyl-4-(trifluoromethyl)-2,3-dihydro-1H-indole (0.130 g, 0.404 mmol; step B above) and NaOH (0.086 g; 2.15 mmol) in MeOH/H2O (4:1; 13 mL) was heated at reflux 3 h. The solvent was removed, the residue was partitioned between Et2O/H2O, and the layers were separated. The aqueous layer was extracted with Et2O (×2). Combined organics were washed (H2O, brine), dried over Na2SO4, filtered and concentrated in vacuo, affording 0.090 g of the title compound as a pale yellow oil which was used without further purification: MS (APCI) m/z 282 (M+H, 81Br).

1. temperaturewas heated
2. temperatureat reflux 3 h
3. customThe solvent was removed
4. customthe residue was partitioned between Et2O/H2O
5. customthe layers were separated
6. extractionThe aqueous layer was extracted with Et2O (×2)
7. washCombined organics were washed (H2O, brine)
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo