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

HRID 2182550

반응식

HRID 2182550 반응식
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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-ecc861c3dbb04a3baa0f9b9cf4f97a41
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06897210B2

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