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product

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

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title product

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

용매

carbitol

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후처리

1. 1
   workup.ADDITIONA mixture of 430 mg
2. 2
   온도to reflux
3. 3
   온도refluxed for 21 hours
4. 4
   온도cooled
5. 5
   여과filtered
6. 6
   workup.ADDITIONThe filtrate was diluted with water
7. 7
   추출extracted well with ethyl acetate
8. 8
   세척The organic phase was washed with brine
9. 9
   건조dried over sodium sulfate
10. 10
    기타evaporated in vacuo
11. 11
    기타The residue was triturated with dichloromethane
12. 12
    여과filtered
13. 13
    기타to remove solid tetrahydrocarbazole
14. 14
    기타The filtrate was evaporated in vacuo

실험 절차

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%.

출처