反应详情

温度

40 °C

Compound of example 8 (224 g) is dissolved in methanol (500 ml) and NaOMe (2 g, 37 mmol) is added. The reaction mixture is stirred at 40° C. for 21/2 h. Methanol (250 ml) is distilled off and CO2 is bubbled through the remaining solution for 5 min reaching pH=7. The reaction mixture is evaporated and isobutyl acetate (450 ml) is added. 50 ml of solvent is evaporated and the resulting mixture is subjected to crystallization by letting it at room temperature for 24 h. The white crystalline solid formed is filtered and washed with tert-butyl methyl ether (200 ml) giving 110 g (73%) of product after drying.

1. distillationMethanol (250 ml) is distilled off
2. customCO2 is bubbled through the remaining solution for 5 min
3. customThe reaction mixture is evaporated
4. additionisobutyl acetate (450 ml) is added
5. custom50 ml of solvent is evaporated
6. customthe resulting mixture is subjected to crystallization
7. customat room temperature
8. customfor 24 h
9. customThe white crystalline solid formed
10. filtrationis filtered
11. washwashed with tert-butyl methyl ether (200 ml)