反应 #2171059

反应方程式

( 1 )

4-(1-tert-Butoxycarbonyl-5-methoxymethyloxy-indol-3-yl)-2-hydroxy-4-oxo-2-butenoic acid methyl ester

lithium hydroxide

→

titled compound

收率 84.0%

4(1-tert-Butoxycarbonyl-5-methoxymethyloxy-indol-3-yl)-2-hydroxy-4-oxo-2-butenoic acid

收率 84.0%

溶剂

dioxane

反应条件

后处理

1. 1
   其他The solvent was removed under reduced pressure at room temperature
2. 2
   workup.DISSOLUTIONthe residue was dissolved in water
3. 3
   洗涤The aqueous layer was washed twice with ethyl acetate and neutralized with 1 N hydrochloric acid (1.7 ml)
4. 4
   萃取extracted with ethyl acetate
5. 5
   洗涤The organic layer was washed with water and brine
6. 6
   其他dried
7. 7
   其他The solvent was removed
8. 8
   洗涤the obtained crystal was washed with ethyl acetate

实验过程

To a solution of 0.345 g (0.85 mmol) of the ester derivative obtained in above (1) in dioxane (7 ml) was added 1.7 ml of 1 N lithium hydroxide. The mixture was stirred for 1.5 hours at room temperature. The solvent was removed under reduced pressure at room temperature and the residue was dissolved in water. The aqueous layer was washed twice with ethyl acetate and neutralized with 1 N hydrochloric acid (1.7 ml) and extracted with ethyl acetate. The organic layer was washed with water and brine, and then dried. The solvent was removed and the obtained crystal was washed with ethyl acetate to give 0.28 g of the titled compound. Yield: 84%. m.p.: 165-170° C. (decomposition)

来源