Cesium carbonate → HCID 57930950、化合物

HRID 1096982ノート

反応式

HRID 1096982 の反応式
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]

参加物

4

反応物 2

HCID 10796Cesium carbonateHCID 57930942HCID 57930942、化合物

生成物 1

HCID 57930950HCID 57930950、化合物

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-74ac28e307c243658e3d40f7cb5af923
出典データセット
uspto-grants-2012_03
特許番号
US08138197B2

反応ノート

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