Trifluoromethanesulfonic anhydride → 4-Cyano-2-methoxyphenyl trifluoromethanesulfonate

HRID 1947236노트

반응식

HRID 1947236 반응식
[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].O[C:17]1[CH:24]=[CH:23][C:20]([C:21]#[N:22])=[CH:19][C:18]=1[O:25][CH3:26]>N1C=CC=CC=1>[F:1][C:2]([F:15])([F:14])[S:3]([O:6][C:17]1[CH:24]=[CH:23][C:20]([C:21]#[N:22])=[CH:19][C:18]=1[O:25][CH3:26])(=[O:5])=[O:4]

참가 물질

4

반응물 2

HCID 67749Trifluoromethanesulfonic anhydrideHCID 781354-Hydroxy-3-methoxybenzonitrile

생성물 1

HCID 166592584-Cyano-2-methoxyphenyl trifluoromethanesulfonate

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

24 ml (141 mmol) of trifluoromethanesulfonic anhydride are slowly added dropwise to a solution of 20 g (134 mmol) of 4-hydroxy-3-methoxybenzonitrile in pyridine (80 ml), keeping the reaction temperature below 25° C. with the aid of an ice bath. The suspension is then stirred at RT for 1 h. Ice-water (400 ml) is added, and the suspension is stirred further until room temperature is reached. It is then filtered, the solid is dissolved in ethyl acetate, and this solution is washed with saturated sodium chloride solution. The organic phase is dried over magnesium sulfate and concentrated. 37.13 g (92% of theory) of the title compound are obtained as a white solid.

후처리

  1. customthe reaction temperature below 25° C.
  2. stirringthe suspension is stirred further until room temperature
  3. filtrationIt is then filtered
  4. dissolutionthe solid is dissolved in ethyl acetate
  5. washthis solution is washed with saturated sodium chloride solution
  6. dry with materialThe organic phase is dried over magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-747b86e4fc784569b72ce5b26dbf25a2
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399471B2

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