反应详情

Reflux a mixture of 5.025 mg (15 mmole) of the 11-chloro ester of Example 14. 3.119 gm of morpholine and 75 ml of acetonitrile for 2 hours. Distill off the acetonitrile under a vacuum and dissolve the residue in 45 ml of methanol at room temperature. Filter, cool and separate the precipitate by filtration. Chromatograph over silica gel eluting with 1:4 ethylacetate in toluene. Recrystallize from ethanol to obtain the title product (m.p. 164°-166° C.).

1. temperatureReflux
2. distillationDistill off the acetonitrile under a vacuum
3. dissolutiondissolve the residue in 45 ml of methanol at room temperature
4. filtrationFilter
5. temperaturecool
6. customseparate the precipitate
7. filtrationby filtration
8. customRecrystallize from ethanol