HCID 21260357、化合物 → 7-(2-Acetoxyethoxy)-4-(2-fluoro-5-hydroxy4-methylanilino)-6-methoxyquinazoline

HRID 634673ノート

反応式

HRID 634673 の反応式
[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[CH:17]=[C:16]2[C:11]([C:12]([NH:18][C:19]3[CH:24]=[C:23]([O:25]CC4C=CC=CC=4)[C:22]([CH3:33])=[CH:21][C:20]=3[F:34])=[N:13][CH:14]=[N:15]2)=[CH:10][C:9]=1[O:35][CH3:36])(=[O:3])[CH3:2].[H][H]>[Pd].C(OCC)(=O)C>[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[CH:17]=[C:16]2[C:11]([C:12]([NH:18][C:19]3[CH:24]=[C:23]([OH:25])[C:22]([CH3:33])=[CH:21][C:20]=3[F:34])=[N:13][CH:14]=[N:15]2)=[CH:10][C:9]=1[O:35][CH3:36])(=[O:3])[CH3:2]

参加物

5

反応物 2

HCID 21260357HCID 21260357、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 212603387-(2-Acetoxyethoxy)-4-(2-fluoro-5-hydroxy4-methylanilino)-6-methoxyquinazoline収率 15%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 7-(2-acetoxyethoxy)-4-(5-benzyloxy-2-fluoro-4-methylanilino)-6-methoxyquinazoline (133 mg, 0.27 mmol) and 10% palladium-on-charcoal catalyst (50 mg) in ethyl acetate (8 ml) was stirred under 1 atmosphere of hydrogen at ambient temperature for 18 hours. The catalyst was removed by filtration through diatomaceous earth and most of the solvent removed by evaporation and hexane added to the residue. The resulting precipitated product was collected by filtration and dried to give 7-(2-acetoxyethoxy)-4-(2-fluoro-5-hydroxy4-methylanilino)-6-methoxyquinazoline (16 mg, 15%).

後処理

  1. customThe catalyst was removed by filtration through diatomaceous earth and most of the solvent
  2. customremoved by evaporation and hexane
  3. additionadded to the residue
  4. customThe resulting precipitated product
  5. filtrationwas collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-c5990c89cade4267922285d9ed2bf45c
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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