反应详情

This compound is prepared by a hydrolysis of the ester from Example 34 as follows: a solution of 0.50 g (0.86 mmole) of the ester, 50 mL of methanol, and 2.0 mL of 1N sodium hydroxide is maintained at reflux for 15 minutes. The methanol is removed, water (30 mL) is added, and 1.0 mL of glacial acetic acid is added to precipitate the gummy product. Purification by silica gel chromatography eluting with 5% methanol-chloroform gives pure product; mp 140°-142° C.

1. temperatureat reflux for 15 minutes
2. customThe methanol is removed
3. additionwater (30 mL) is added
4. addition1.0 mL of glacial acetic acid is added
5. customto precipitate the gummy product
6. customPurification by silica gel chromatography
7. washeluting with 5% methanol-chloroform
8. customgives pure product