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

HRID 279651ノート

反応式

HRID 279651 の反応式
[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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

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-amino4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)quinazoline hydrochloride (4.8 g, 97%) as a yellow solid.

後処理

  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

出典と根拠

ORDレコード
ord-d287aec569004237b2bef94e72672fc3
出典データセット
uspto-grants-2002_03
特許番号
US06362336B1

反応ノート

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