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

HRID 657995ノート

反応式

HRID 657995 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-d07d88d9940b41279189d6115787ecea
出典データセット
uspto-grants-2011_12
特許番号
US08076336B2

反応ノート

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