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Triethylamine → Methanesulfonic acid 2-[5-(4-bromo-phenyl)-3-methyl-isoxazol-4-yl]ethyl ester

HRID 1512594
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반응식

HRID 1512594 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:12][N:11]=[C:10]([CH3:13])[C:9]=2[CH2:14][CH2:15][OH:16])=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:24][S:25](Cl)(=[O:27])=[O:26]>C1COCC1.O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[O:12][N:11]=[C:10]([CH3:13])[C:9]=2[CH2:14][CH2:15][O:16][S:25]([CH3:24])(=[O:27])=[O:26])=[CH:6][CH:7]=1
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 665772962-[5-(4-Bromo-phenyl)-3-methyl-isoxazol-4-yl]-ethanol

생성물 1

HCID 86652398Methanesulfonic acid 2-[5-(4-bromo-phenyl)-3-methyl-isoxazol-4-yl]ethyl ester

시약·촉매·용매 2

HCID 962Water용매HCID 8028
Tetrahydrofuran
용매

반응 조건

온도
0 °C

실험 절차

To a solution of 2-[5-(4-bromo-phenyl)-3-methyl-isoxazol-4-yl]-ethanol (0.100 g, 0.35 mmol) and triethylamine (0.10 mL, 0.71 mmol) in THF at 0° C. was added methanesulfonyl chloride (0.05 mL, 0.62 mmol) and the reaction stirred at 0° C. for 1 hour. The mixture was diluted with H2O and extracted with EtOAc, and the combined organic layers were washed with H2O, saturated aqueous NaHCO3, and brine. Dried over MgSO4, filtered, and concentrated to give the title compound.

후처리

  1. extractionextracted with EtOAc
  2. washthe combined organic layers were washed with H2O, saturated aqueous NaHCO3, and brine
  3. dry with materialDried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-bd286ca53d414897ab6998f1fb81bc2b
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08217066B2

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