[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

反応式

HRID 51310 の反応式
[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

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8146Diethylene Glycol Monoethyl Ether溶媒

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%.

後処理

  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

出典と根拠

ORDレコード
ord-1987d5e7313946f0bcb447800840db56
出典データセット
uspto-grants-2004_03
特許番号
US06713645B1

関連ノート

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