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Trimethylsilyl triflate → HCID 86675228、化合物

HRID 1502912
ノート
印刷プレビュー

反応式

HRID 1502912 の反応式
[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([C:12](=[O:14])[CH3:13])=[CH:8][CH:7]=2)[CH:5]=[N:4][CH:3]=[N:2]1.FC(F)(F)S(O[Si:21]([CH3:24])([CH3:23])[CH3:22])(=O)=O>C(Cl)Cl>[CH3:22][Si:21]([CH3:24])([CH3:23])[O:14][C:12]([C:9]1[CH:8]=[CH:7][C:6]([N:1]2[CH:5]=[N:4][CH:3]=[N:2]2)=[CH:11][CH:10]=1)=[CH2:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 65367Trimethylsilyl triflateHCID 25603171-[4-(1H-1,2,4-Triazol-1-yl)phenyl]ethan-1-one

生成物 1

HCID 86675228HCID 86675228、化合物収率 88.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 1-(4-(1H-1,2,4-triazol-1-yl)phenyl)ethanone (4.5 g, 24.0 mmol) in CH2Cl2 at 0° C., were added TEA (3.7 g, 36.1 mmol) and trimethylsilyl trifluoromethanesulfonate (8 g, 36 mmol) and the resultant reaction mixture was stirred for 1 h. The reaction mixture was quenched with a mixture of sat aq sodium bicarbonate solution and ether. The ether layer and was separated, washed with brine, dried over Na2SO4 and concentrated under reduced pressure to afford the title compound (5.5 g) which was taken directly to next step.

後処理

  1. customthe resultant reaction mixture
  2. customThe reaction mixture was quenched with a mixture of sat aq sodium bicarbonate solution and ether
  3. customThe ether layer and was separated
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-5b2acd3aef95439fb9d2fb7c8795e71c
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09211280B2

反応ノート

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