Cesium carbonate → HCID 57930950, 화합물

HRID 1096982노트

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HRID 1096982 반응식
C(=O)([O-])[O-].[Cs+].[Cs+].[Br:7][C:8]1[C:17]([O:18][S:19]([C:22]([F:25])([F:24])[F:23])(=[O:21])=[O:20])=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[CH:10][C:9]=1[O:26]S(C(F)(F)F)(=O)=O>COCCOC>[Br:7][C:8]1[C:17]([O:18][S:19]([C:22]([F:23])([F:24])[F:25])(=[O:20])=[O:21])=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[CH:10][C:9]=1[OH:26]

참가 물질

4

반응물 2

HCID 10796Cesium carbonateHCID 57930942HCID 57930942, 화합물

생성물 1

HCID 57930950HCID 57930950, 화합물

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
60 °C

실험 절차

In a 1-liter egg plant-type flask, cesium carbonate (24.8 g, 76.3 mmol) was added to a DME (200 mL) solution of methyl 4-bromo-3,5-bis{[(trifluoromethyl)sulfonyl]oxy}benzoate (26.0 g), and stirred at 60° C. for 3 hours. DME was removed under reduced pressure, the residue was diluted with ethyl acetate, washed with water and saturated saline water in that order, dried with sodium sulfate, filtered and concentrated to obtain a crude product as a brown solid. This was washed with a mixed solvent of toluene and hexane to obtain the title compound as a colorless solid.

후처리

  1. customDME was removed under reduced pressure
  2. additionthe residue was diluted with ethyl acetate
  3. washwashed with water and saturated saline water in that order
  4. dry with materialdried with sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto obtain a crude product as a brown solid
  8. washThis was washed with a mixed solvent of toluene and hexane

출처 및 근거

ORD 기록
ord-74ac28e307c243658e3d40f7cb5af923
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08138197B2

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