反应详情

A mixture of Step 1 intermediate (17 g, 97.34 mmol) and hydrazine hydrate (119 ml) in isopropyl alcohol (280 ml) were refluxed for 1 h. The excess of solvent was removed under reduced pressure, solid obtained was filtered, washed with methanol (25 ml) and dried to obtain 8.1 g of the product as white solid; 1H NMR (300 MHz, DMSO-d6): δ 3.09 (s, 3H), 3.21 (s, 3H), 4.37 (br s, 2H), 5.10 (s, 1H), 8.02 (br s, 1H).

1. customThe excess of solvent was removed under reduced pressure, solid
2. customobtained
3. filtrationwas filtered
4. washwashed with methanol (25 ml)
5. customdried