Trifluoromethanesulfonic anhydride → Pyridin-4-yl trifluoromethanesulfonate

HRID 2209094노트

반응식

HRID 2209094 반응식
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]

참가 물질

4

반응물 2

HCID 67749Trifluoromethanesulfonic anhydrideHCID 178504229HCID 178504229, 화합물

생성물 1

HCID 18424478Pyridin-4-yl trifluoromethanesulfonate수율 123.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f56aa9bd71e64ea78772f7fc41e78be0
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09376441B2

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