反应详情

A mixture of 430C (1.60 g, 3.73 mmol) and 6N NaOH (5 ml, 30 mmol) in a mixed solvent of MeOH/THF (20 ml, 1/1) was heated at reflux for 2 h, cooled to rt. Removed half of the solvent in vacuo. The residue was treated with H2O (30 ml), washed with CH2Cl2 (3×50 ml). The aqueous layer was acidified to PH=5 and extracted with EtOAc (3×50 ml). The combined organic layers were washed with H2O (2×30 ml) and brine (30 ml), dried with Na2SO4. Removal of the solvent under reduced pressure gave 430D (1.47 g, 95%) as a yellow powder. It has retention time of 5.88 min (∠Cl, 8 min. run). MS Found: (M+H)+=415.2.

1. temperaturewas heated
2. temperatureat reflux for 2 h
3. customRemoved half of the solvent in vacuo
4. additionThe residue was treated with H2O (30 ml)
5. washwashed with CH2Cl2 (3×50 ml)
6. extractionextracted with EtOAc (3×50 ml)
7. washThe combined organic layers were washed with H2O (2×30 ml) and brine (30 ml)
8. dry with materialdried with Na2SO4
9. customRemoval of the solvent under reduced pressure