Water → Methyl 3-methoxy-5-(trifluoromethyl)benzoate

HRID 217748ノート

反応式

HRID 217748 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1)[C:5](O)=[O:6].CI.[C:17](=O)([O-])[O-].[K+].[K+].O.CN([CH:27]=[O:28])C>>[CH3:17][O:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1)[C:5]([O:28][CH3:27])=[O:6]

参加物

6

反応物 5

HCID 962WaterHCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27831463-hydroxy-5-(trifluoromethyl)benzoic Acid

生成物 1

HCID 46311161Methyl 3-methoxy-5-(trifluoromethyl)benzoate

実験手順

3-Hydroxy-5-trifluoromethylbenzoic acid (2 g) was initially charged at RT in DMF (15 ml) while stirring, and admixed dropwise with methyl iodide (3.0 ml). After adding potassium carbonate (5.6 g), the mixture was stirred for 5 h and left to stand overnight. It was then admixed with water and extracted three times with MtB ether. The combined MTB ether phases were dried over sodium sulfate, filtered and concentrated. 2.29 g of the title compound were obtained.

後処理

  1. stirringthe mixture was stirred for 5 h
  2. waitleft
  3. extractionextracted three times with MtB ether
  4. dry with materialThe combined MTB ether phases were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-6ec8dcf9d8e141738b0b38ed3d53305f
出典データセット
uspto-grants-2012_06
特許番号
US08198272B2

反応ノート

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