Dimethylformamide → HCID 54576351、化合物

HRID 1096946ノート

反応式

HRID 1096946 の反応式
[C:1](=O)([O-])[O-].[K+].[K+].IC.CN(C=O)C.[OH:14][C:15]1[CH:16]=[C:17]([CH:22]=[C:23]([O:25][S:26]([C:29]([F:32])([F:31])[F:30])(=[O:28])=[O:27])[CH:24]=1)[C:18]([O:20][CH3:21])=[O:19]>C(OCC)C>[CH3:1][O:14][C:15]1[CH:16]=[C:17]([CH:22]=[C:23]([O:25][S:26]([C:29]([F:32])([F:30])[F:31])(=[O:28])=[O:27])[CH:24]=1)[C:18]([O:20][CH3:21])=[O:19]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86635508HCID 86635508、化合物

生成物 1

HCID 54576351HCID 54576351、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

With cooling with ice, potassium carbonate (152 mg, 1.10 mmol) and iodomethane (0.137 mL, 2.20 mmol) were added to a DMF solution (3.0 mL) of methyl 3-hydroxy-5-trifluoromethane-sulfonyloxybenzoate (300 mg, 1.00 mmol), and stirred at room temperature for 17 hours. The reaction mixture was diluted with diethyl ether (30 mL), washed with water and aqueous saturated sodium chloride solution, dried with sodium sulfate, and concentrated under reduced pressure. The residue was purified through silica gel column chromatography to obtain the title compound as a colorless oil.

後処理

  1. washwashed with water and aqueous saturated sodium chloride solution
  2. dry with materialdried with sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified through silica gel column chromatography

出典と根拠

ORDレコード
ord-49b0f8a3149c4f5b803e9a2a5fb9294a
出典データセット
uspto-grants-2012_03
特許番号
US08138197B2

反応ノート

読み込み中…