Methanol → 4-(4-Bromo-2-fluoroanilino)6-methoxy-7-(3-methylsulphonylpropoxy)quinazoline

HRID 2182550

反応式

HRID 2182550 の反応式
O[O:2][S:3]([O-:5])=O.[K+].[Br:7][C:8]1[CH:32]=[CH:31][C:11]([NH:12][C:13]2[C:22]3[C:17](=[CH:18][C:19]([O:25][CH2:26][CH2:27][CH2:28]SC)=[C:20]([O:23][CH3:24])[CH:21]=3)[N:16]=[CH:15][N:14]=2)=[C:10]([F:33])[CH:9]=1.[CH3:34]O>O.C(Cl)Cl>[Br:7][C:8]1[CH:32]=[CH:31][C:11]([NH:12][C:13]2[C:22]3[C:17](=[CH:18][C:19]([O:25][CH2:26][CH2:27][CH2:28][S:3]([CH3:34])(=[O:5])=[O:2])=[C:20]([O:23][CH3:24])[CH:21]=3)[N:16]=[CH:15][N:14]=2)=[C:10]([F:33])[CH:9]=1

参加物

6

反応物 3

HCID 887MethanolHCID 224782814-(4-Bromo-2-fluoroanilino)-6-methoxy-7-(3-methylthiopropoxy)quinazolineHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 187534474-(4-Bromo-2-fluoroanilino)6-methoxy-7-(3-methylsulphonylpropoxy)quinazoline収率 73%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of OXONE, (trade mark of E.I. du Pont de Nemours & Co., Inc), (800 mg) in water (4.5 ml) was added to a solution of 4-(4-bromo-2-fluoroanilino)-6-methoxy-7-(3 methylthiopropoxy)quinazoline (300 mg, 0.66 mmol), (prepared as described in Example 31), in methanol (15 ml) and the mixture was stirred for 4 hours at ambient temperature. The mixture was diluted with methylene chloride, was washed with aqueous sodium hydrogen carbonate solution, dried (MgSO4) and the solvent was removed by evaporation. The residue was triturated with ethyl acetate/hexane, collected by filtration and dried to give 4-(4-bromo-2-fluoroanilino)6-methoxy-7-(3-methylsulphonylpropoxy)quinazoline (235 mg, 73%).

後処理

  1. washwas washed with aqueous sodium hydrogen carbonate solution
  2. dry with materialdried (MgSO4)
  3. customthe solvent was removed by evaporation
  4. customThe residue was triturated with ethyl acetate/hexane
  5. filtrationcollected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-ecc861c3dbb04a3baa0f9b9cf4f97a41
出典データセット
uspto-grants-2005_05
特許番号
US06897210B2

関連ノート

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