Trifluoromethanesulfonic anhydride → Pyridin-4-yl trifluoromethanesulfonate

HRID 2209094ノート

反応式

HRID 2209094 の反応式
C[Si](C)(C)CCOCN1C=C([C:12]2[CH:17]=[C:16]([OH:18])[CH:15]=[CH:14][N:13]=2)C=N1.[O:21](S(C(F)(F)F)(=O)=O)[S:22]([C:25]([F:28])([F:27])[F:26])(=O)=[O:23]>C(Cl)Cl>[F:26][C:25]([F:28])([F:27])[S:22]([O:18][C:16]1[CH:15]=[CH:14][N:13]=[CH:12][CH:17]=1)(=[O:23])=[O:21]

参加物

4

反応物 2

HCID 67749Trifluoromethanesulfonic anhydrideHCID 178504229HCID 178504229、化合物

生成物 1

HCID 18424478Pyridin-4-yl trifluoromethanesulfonate収率 123.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To solution of 2-(1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazol-4-yl)pyridin-4-ol (0.67 g, 2 mmol) in DCM was added TEA (0.69 g, 7 mmol) and the mixture was stirred at OC, (Tf)2O (0.843 g, 3 mmol) was added slowly. The resulting reaction mixture was steered at r.t. for one hour. Solvent was removed under vacuo. And the residue was purified by silicone gel column to afford 2414(2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazol-4-yl)pyridin-4-yl trifluoromethanesulfonate (0.56 g, 58%) LCMS-ESI+ (m/z): [M+H]+ calcd. for C26H30N5O3: 424.48; found: 424.05.

後処理

  1. additionwas added slowly
  2. customThe resulting reaction mixture
  3. customSolvent was removed under vacuo
  4. customAnd the residue was purified by silicone gel column

出典と根拠

ORDレコード
ord-f56aa9bd71e64ea78772f7fc41e78be0
出典データセット
uspto-grants-2016_06
特許番号
US09376441B2

反応ノート

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