Methanol → HCID 54565608、化合物

HRID 1288695ノート

反応式

HRID 1288695 の反応式
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

参加物

4

反応物 2

HCID 887MethanolHCID 18924611HCID 18924611、化合物

生成物 1

HCID 54565608HCID 54565608、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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-methanesulphonylphenyl)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).

後処理

  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

出典と根拠

ORDレコード
ord-6308dce326a54e1d847d6250cc7a947a
出典データセット
uspto-grants-1998_05
特許番号
US05747424

反応ノート

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