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HCID 19853360, 화합물 → HCID 19853335, 화합물

HRID 1607300
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HRID 1607300 반응식
C([O:8][C:9]1[C:10]([F:30])=[C:11]([F:29])[CH:12]=[C:13]2[C:18]=1[N:17]([NH:19][CH2:20][CH:21]=[O:22])[CH:16]=[C:15]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:14]2=[O:28])C1C=CC=CC=1>C(Cl)(Cl)Cl.CO.[Pd]>[F:29][C:11]1[CH:12]=[C:13]2[C:18](=[C:9]([OH:8])[C:10]=1[F:30])[N:17]([NH:19][CH2:20][CH:21]=[O:22])[CH:16]=[C:15]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:14]2=[O:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 19853360HCID 19853360, 화합물

생성물 1

HCID 19853335HCID 19853335, 화합물수율 92.4%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 6212Chloroform용매

실험 절차

Ethyl 8-benzyloxy-6,7-difluoro-1-(formylmethylamino)-4-oxo-1,4-dihydro-3-quinolinecarboxylate (330 mg) was hydrogenated over 5% Pd/C (50 mg) in chloroform (14 ml) for 4 hours. The reaction mixture was diluted with methanol (14 ml) and filtered. The filtered cake was washed with chloroform/methanol (1:1). The combined filtrate was evaporated and the residue was recrystallized from ethanol to give 239 mg of ethyl 6,7-difluoro-1-(formylmethylamino)-8-hydroxy-4-oxo-1,4-dihydro-3-quinolinecarboxylate, mp 221°-225° C. (dec.); MS m/z 326 (M+).

후처리

  1. filtrationfiltered
  2. washThe filtered cake was washed with chloroform/methanol (1:1)
  3. customThe combined filtrate was evaporated
  4. customthe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-6314d52854524c3ebb019c30e76b1ecc
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04864023

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