HCID 57287670, 화합물 → Eltenac

HRID 1680165노트

반응식

HRID 1680165 반응식
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

참가 물질

6

반응물 2

HCID 57287670HCID 57287670, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 51717Eltenac

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 176Acetic Acid용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4555f856d4334156aca82e16b1baa2ab
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04272507

반응 노트

불러오는 중…