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

HRID 51310

반응식

HRID 51310 반응식
[Na+].[CH2:2]([N:9]1[C:21]2[CH2:20][CH2:19][CH2:18][CH:17]([C:22](=[O:24])[NH2:23])[C:16]=2[C:15]2[C:10]1=[CH:11][C:12]([O:30][CH3:31])=[CH:13][C:14]=2[O:25][CH2:26][C:27]([O-:29])=[O:28])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>[Pd].CCOCCOCCO>[CH2:2]([N:9]1[C:21]2[CH:20]=[CH:19][CH:18]=[C:17]([C:22](=[O:24])[NH2:23])[C:16]=2[C:15]2[C:10]1=[CH:11][C:12]([O:30][CH3:31])=[CH:13][C:14]=2[O:25][CH2:26][C:27]([OH:29])=[O:28])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

4

반응물 1

HCID 23676539[9-Benzyl-4-carbamoyl-7-methoxy-1,2,3,4-tetrahydrocarbazol-5-yl]oxyacetic acid sodium salt

생성물 1

HCID 10135839[9-Benzyl-4-carbamoyl-7-methoxycarbazol-5-yl]oxyacetic acid

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8146Diethylene Glycol Monoethyl Ether용매

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%.

후처리

  1. additionA mixture of 430 mg
  2. temperatureto reflux
  3. temperaturerefluxed for 21 hours
  4. temperaturecooled
  5. filtrationfiltered
  6. additionThe filtrate was diluted with water
  7. extractionextracted well with ethyl acetate
  8. washThe organic phase was washed with brine
  9. dry with materialdried over sodium sulfate
  10. customevaporated in vacuo
  11. customThe residue was triturated with dichloromethane
  12. filtrationfiltered
  13. customto remove solid tetrahydrocarbazole
  14. customThe filtrate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-1987d5e7313946f0bcb447800840db56
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06713645B1

연결된 노트

불러오는 중…