反应详情

Compound 29 (2.21 g, 10 mM) in methanol (150 ml) containing Et3N (2 ml) was treated with 4-methoxyphenylhydrazine hydrochloride (1.85 g, 10.6 mM) at RT for 4 hr. The solvent was removed in vacuo and the residue was partitioned between 5% NaOH and Et2O. The basic aqueous layer was separated and acidified with 10% HCl to pH 2. Saturated brine was added and the aqueous layer was exhaustively extracted with CH2Cl2. The combined CH2Cl2 layers were concentrated to give the title compound 31 as a tan crystalline solid (Recry. Acetone, 1.87 g, 52%) mp=226°-228° C., MS, m/e 323 (M+).

1. customThe solvent was removed in vacuo
2. customthe residue was partitioned between 5% NaOH and Et2O
3. customThe basic aqueous layer was separated
4. additionSaturated brine was added
5. extractionthe aqueous layer was exhaustively extracted with CH2Cl2
6. concentrationThe combined CH2Cl2 layers were concentrated