Methanol → 7-Amino4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)quinazoline hydrochloride

HRID 1421043노트

반응식

HRID 1421043 반응식
[ClH:1].[F:2][C:3]1[CH:22]=[C:21]([CH3:23])[C:20]([O:24][C:25]([O:27][CH3:28])=[O:26])=[CH:19][C:4]=1[NH:5][C:6]1[C:15]2[C:10](=[CH:11][C:12]([N+:16]([O-])=O)=[CH:13][CH:14]=2)[N:9]=[CH:8][N:7]=1.CO>[Pd].C(O)C.Cl>[ClH:1].[NH2:16][C:12]1[CH:11]=[C:10]2[C:15]([C:6]([NH:5][C:4]3[CH:19]=[C:20]([O:24][C:25]([O:27][CH3:28])=[O:26])[C:21]([CH3:23])=[CH:22][C:3]=3[F:2])=[N:7][CH:8]=[N:9]2)=[CH:14][CH:13]=1

참가 물질

6

반응물 2

HCID 887MethanolHCID 226250474-(2-Fluoro-5-methoxycarbonyloxy-4-methylanilino)7-nitroquinazoline hydrochloride

생성물 1

HCID 226250847-Amino4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)quinazoline hydrochloride수율 97.5%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

A mixture of 4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)-7-nitroquinazoline hydrochloride (5.3 g, 13 mmol) and 10% palladium-on-charcoal catalyst (1 g) in ethanol (100 ml), ethanolic hydrogen chloride (1.8 ml of a 7M solution) and methanol (20 ml) was stirred under hydrogen at 1.7 atmospheres pressure for 75 minutes. The catalyst was removed by filtration through diatomaceous earth and the filter pad thoroughly washed with methylene chloride, methanol and ether and the solvent was removed from the filtrate by evaporation to give 7-amino-4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)quinazoline hydrochloride (4.8 g, 97%) as a yellow solid.

후처리

  1. customThe catalyst was removed by filtration through diatomaceous earth
  2. washthe filter pad thoroughly washed with methylene chloride, methanol and ether
  3. customthe solvent was removed from the filtrate by evaporation

출처 및 근거

ORD 기록
ord-220a3d8ba40547c6b96669e2bc58ffe2
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06071921

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