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

HRID 634744ノート

反応式

HRID 634744 の反応式
[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]

参加物

5

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-9b3cd4a76e4c47dd8006335f5e48e243
出典データセット
uspto-grants-2001_02
特許番号
US06184225B2

反応ノート

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