HCID 57287670、化合物 → Eltenac

HRID 1680165ノート

反応式

HRID 1680165 の反応式
C([O:8][C:9](=[O:25])[CH2:10][C:11]1[C:15]([NH:16][C:17]2[C:22]([Cl:23])=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:24])=[CH:14][S:13][CH:12]=1)C1C=CC=CC=1.[H][H]>C(OCC)(=O)C.C(O)(=O)C.[Pd]>[Cl:24][C:18]1[CH:19]=[CH:20][CH:21]=[C:22]([Cl:23])[C:17]=1[NH:16][C:15]1[C:11]([CH2:10][C:9]([OH:25])=[O:8])=[CH:12][S:13][CH:14]=1

参加物

6

反応物 2

HCID 57287670HCID 57287670、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 51717Eltenac

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

393 mg (1 mmole) of 4-(2,6-dichloroanilino)-3-thiophenacetic acid benzyl ester are subjected to hydrogenolysis (in a mixture of 100 ml of ethyl acetate and 10 ml of glacial acetic acid in a circulatory hydrogenation apparatus in the presence of 50 mg of 10 percent strength palladium-on-active charcoal at room temperature and under atmospheric pressure) until the theoretical amount of hydrogen has been taken up. The catalyst is filtered off, the filtrate is concentrated in vacuo, and the residue is dissolved in 1 N sodium hydroxide solution. The aqueous solution is extracted with toluene, and the product phase is acidified with 1 N hydrochloric acid and extracted again with toluene. The organic phase is dried and concentrated. 4-(2,6-Dichloroanilino)-3-thiophenacetic acid (m. 179° to 180°) is obtained.

後処理

  1. filtrationThe catalyst is filtered off
  2. concentrationthe filtrate is concentrated in vacuo
  3. dissolutionthe residue is dissolved in 1 N sodium hydroxide solution
  4. extractionThe aqueous solution is extracted with toluene
  5. extractionextracted again with toluene
  6. customThe organic phase is dried
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-4555f856d4334156aca82e16b1baa2ab
出典データセット
uspto-grants-1981_06
特許番号
US04272507

反応ノート

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