反应详情

Stir a mixture of 1.77 gm. (5 mmole) of the ester of Example 11, 1.12 gm. (10 mmole) of 85% aqueous potassium hydroxide, 5.5 ml. of water, 27.5 ml. of ethanol and 2.75 ml. of dioxane under argon at room temperature for 21/2 hours. Evaporate to a small volume and dilute with 18 ml. of water. Filter and acidify with acetic acid to pH 4.5. Separate the precipitate by filtration, wash with water and dry in vacuo over calcium chloride. Recrystallize from acetonitrile to obtain the title product, (m.p. 267°-269° C.).

1. additiona mixture of 1.77 gm
2. customat room temperature
3. custom2 hours
4. customEvaporate to a small volume
5. additiondilute with 18 ml
6. filtrationFilter
7. customSeparate the precipitate
8. filtrationby filtration
9. washwash with water
10. dry with materialdry in vacuo over calcium chloride
11. customRecrystallize from acetonitrile