反应详情

Add 269 mg. (1 mmole) of the ester of Example 9 to a solution of 132 mg. (2 mmole) of 85% aqueous potassium hydroxide in a mixture of 6.5 ml. of ethanol, 0.65 ml. of dioxane and 1.3 ml. of water. Stir at room temperature for 2 hours. Filter and evaporate the solution to a small volume. Dilute with 9 ml. of water and acidify with acetic acid. Filter wash the solids with water and dry. Dissolve the product in 9 ml. of hot tetrahydrofuran, filter and dilute with 9 ml. of methanol. Evaporate to a thick slurry, dilute with 2 ml. of methanol, filter and wash with methanol. Dry to obtain the title product, (m.p. sinters 289° C., m.p. 290°-291° C. dec.).

1. additionAdd 269 mg
2. filtrationFilter
3. customevaporate the solution to a small volume
4. additionDilute with 9 ml
5. filtrationFilter
6. washwash the solids with water
7. customdry
8. dissolutionDissolve the product in 9 ml
9. filtrationof hot tetrahydrofuran, filter
10. additiondilute with 9 ml
11. customEvaporate to a thick slurry
12. additiondilute with 2 ml
13. filtrationof methanol, filter
14. washwash with methanol
15. customDry