Methanol → HCID 54565608, 화합물

HRID 266509노트

반응식

HRID 266509 반응식
Br[CH:2]([C:11]1[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:19])=[O:18])=[CH:13][C:12]=1[Cl:21])[C:3]1[CH:4]=[N:5][O:6][C:7]=1[CH:8]1[CH2:10][CH2:9]1.[CH3:22][OH:23]>C1(C)C=CC=CC=1>[CH3:22][O:23][CH:2]([C:11]1[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:19])=[O:18])=[CH:13][C:12]=1[Cl:21])[C:3]1[CH:4]=[N:5][O:6][C:7]=1[CH:8]1[CH2:10][CH2:9]1

참가 물질

4

반응물 2

HCID 887MethanolHCID 18924611HCID 18924611, 화합물

생성물 1

HCID 54565608HCID 54565608, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 4-[bromo-(2-chloro-4-methanesulphonylphenyl)-methyl]-5-cyclopropylisoxazole (2.5 g) and methanol (2.0 ml) in toluene was stirred at reflux for 16 hours. The resultant solution was evaporated to dryness and the residue was dissolved in ethyl acetate. This solution was washed with water, dried (MgSO4), and filtered. The filtrate was evaporated to dryness. The residue was purified by chromatography on silica eluted with ethyl acetate and petroleum ether to give 4-[methoxy-(2-chloro-4-methanesulphonyl-phenyl)methyl]-5-cyclopropylisoxazole (compound 307, 1.40 g) as a colourless oil, NMR: (CDCl3) 1.0(4H, m), 2.1 (1H, m), 3.0(3H,s), 3.3(3H, s), 5.6(1H,s), 7.9(4H,m).

후처리

  1. temperatureat reflux for 16 hours
  2. customThe resultant solution was evaporated to dryness
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThis solution was washed with water
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness
  8. customThe residue was purified by chromatography on silica
  9. washeluted with ethyl acetate and petroleum ether

출처 및 근거

ORD 기록
ord-18663e0cddaa43dfbc294db17d283248
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05650533

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