反応 #79588

反応方程式

product

[9-benzyl-4-carbamoyl-7-methoxy-1,2,3,4-tetrahydrocarbazol-5-yl]oxyacetic acid sodium salt

→

title product

[9-benzyl-4-carbamoyl-7-methoxycarbazol-5-yl]oxyacetic acid

溶媒

carbitol

反応条件

後処理

1. 1
   workup.ADDITIONA mixture of 430 mg
2. 2
   温度to reflux
3. 3
   温度refluxed for 21 hours
4. 4
   温度cooled
5. 5
   ろ過filtered
6. 6
   workup.ADDITIONThe filtrate was diluted with water
7. 7
   抽出extracted well with ethyl acetate
8. 8
   洗浄The organic phase was washed with brine
9. 9
   乾燥dried over sodium sulfate
10. 10
    その他evaporated in vacuo
11. 11
    その他The residue was triturated with dichloromethane
12. 12
    ろ過filtered
13. 13
    その他to remove solid tetrahydrocarbazole
14. 14
    その他The filtrate was evaporated in vacuo

実験手順

A mixture of 430 mg. of the product from Example 3 Part D, 2.0 gm. of 5% Pd/C, and 20 mL of carbitol was heated to reflux and refluxed for 21 hours, cooled, and filtered. The filtrate was diluted with water, acidified with hydrochloric acid, and extracted well with ethyl acetate. The organic phase was washed with brine, dried over sodium sulfate and evaporated in vacuo. The residue was triturated with dichloromethane and filtered to remove solid tetrahydrocarbazole. The filtrate was evaporated in vacuo to give the title product, 125 mg, 31%.

出典