反应详情

Using the procedure of Example 2, 3 g of the product of Example 22, 70 ml of methanol and 17 ml of 2N hydrochloric were reacted and the solution was refluxed for 90 minutes. It was poured into 200 ml of ammonium hydroxide +100 g of ice saturated with sodium chloride and extraction was carried out 4 times with ethyl acetate. The extracts were washed with salt water, dried and purified on silica with methylene chloride-methanol: 9-1 as eluant. After crystallization from methylene chloride-isopropyl ether, 2.12 g of the expected product (white crystals) melting at 188-189° C. were obtained.

1. customhydrochloric were reacted
2. temperaturethe solution was refluxed for 90 minutes
3. washThe extracts were washed with salt water
4. customdried
5. custompurified on silica with methylene chloride-methanol
6. customAfter crystallization from methylene chloride-isopropyl ether