4-(2-Fluoro-5-methoxycarbonyloxy-4-methylanilino)-6-methoxy-7-nitroquinazoline hydrochloride → 7-Amino4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)-6-methoxyquinazoline hydrochloride

HRID 634744노트

반응식

HRID 634744 반응식
[ClH:1].[F:2][C:3]1[CH:24]=[C:23]([CH3:25])[C:22]([O:26][C:27]([O:29][CH3:30])=[O:28])=[CH:21][C:4]=1[NH:5][C:6]1[C:15]2[C:10](=[CH:11][C:12]([N+:18]([O-])=O)=[C:13]([O:16][CH3:17])[CH:14]=2)[N:9]=[CH:8][N:7]=1>[Pd].CO.C(O)C>[ClH:1].[NH2:18][C:12]1[CH:11]=[C:10]2[C:15]([C:6]([NH:5][C:4]3[CH:21]=[C:22]([O:26][C:27]([O:29][CH3:30])=[O:28])[C:23]([CH3:25])=[CH:24][C:3]=3[F:2])=[N:7][CH:8]=[N:9]2)=[CH:14][C:13]=1[O:16][CH3:17]

참가 물질

5

반응물 1

HCID 212603424-(2-Fluoro-5-methoxycarbonyloxy-4-methylanilino)-6-methoxy-7-nitroquinazoline hydrochloride

생성물 1

HCID 212603307-Amino4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)-6-methoxyquinazoline hydrochloride수율 91%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

A mixture of 4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)-6-methoxy-7-nitroquinazoline hydrochloride (1.1 g, 25 mmol) and 10% palladium-on-charcoal catalyst (220 mg) in methanol (200 ml) and ethanol (10 ml) was stirred under hydrogen at 2.7 atmospheres for 7 hours. The catalyst was removed by filtration through diatomaceous earth, the solvent removed from the filtrate by evaporation and the solid residue washed with ether, collected by filtration and dried under vacuum to give 7-amino4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)-6-methoxyquinazoline hydrochloride (930 mg, 91%).

후처리

  1. customThe catalyst was removed by filtration through diatomaceous earth
  2. customthe solvent removed from the filtrate by evaporation
  3. washthe solid residue washed with ether
  4. filtrationcollected by filtration
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-9b3cd4a76e4c47dd8006335f5e48e243
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06184225B2

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