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

HRID 1477602
ノート
印刷プレビュー

反応式

HRID 1477602 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b8f01f2fa8b2467599ea3a2da4c36872
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09403798B2

反応ノート

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