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Triethylamine → [5-(2,2,2-Trifluoroethoxy)pyridin-2-yl]methyl methanesulfonate

HRID 1477602
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HRID 1477602 반응식
[F:1][C:2]([F:14])([F:13])[CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([CH2:11][OH:12])=[N:9][CH:10]=1.C(N(CC)CC)C.[CH3:22][S:23](Cl)(=[O:25])=[O:24]>ClCCl>[CH3:22][S:23]([O:12][CH2:11][C:8]1[CH:7]=[CH:6][C:5]([O:4][CH2:3][C:2]([F:1])([F:13])[F:14])=[CH:10][N:9]=1)(=[O:25])=[O:24]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 66893281(5-(2,2,2-Trifluoroethoxy)pyridin-2-yl)methanol

생성물 1

HCID 117839939[5-(2,2,2-Trifluoroethoxy)pyridin-2-yl]methyl methanesulfonate수율 67.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a dichloromethane solution (2.8 mL) of [5-(2,2,2-trifluoroethoxy)pyridin-2-yl]methanol (138 mg, 0.67 mmol), triethylamine (468 μL, 3.33 mmol) and methanesulfonyl chloride (77.4 μL, 1.00 mmol) were added at 0° C. and the resultant solution was stirred for 30 minutes. After completion of the reaction, the reaction solution was washed with saturated ammonium chloride aqueous solution and brine. The obtained organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain a crude product (129 mg) of the title compound.

후처리

  1. customAfter completion of the reaction
  2. washthe reaction solution was washed with saturated ammonium chloride aqueous solution and brine
  3. dry with materialThe obtained organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b8f01f2fa8b2467599ea3a2da4c36872
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09403798B2

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