Toluene → Methyl 2,5-bis(2,2,2-trifluoroethoxy)benzoate

HRID 460427

反応式

HRID 460427 の反応式
[F:1][C:2]([F:21])([F:20])[CH2:3][O:4][C:5]1[CH:13]=[CH:12][C:11]([O:14][CH2:15][C:16]([F:19])([F:18])[F:17])=[CH:10][C:6]=1[C:7]([OH:9])=[O:8].S(Cl)(Cl)=O.[C:26]1(C)C=CC=CC=1>CO>[F:1][C:2]([F:20])([F:21])[CH2:3][O:4][C:5]1[CH:13]=[CH:12][C:11]([O:14][CH2:15][C:16]([F:19])([F:18])[F:17])=[CH:10][C:6]=1[C:7]([O:9][CH3:26])=[O:8]

参加物

5

反応物 3

HCID 1140TolueneHCID 24386Thionyl ChlorideHCID 27360782,5-bis(2,2,2-trifluoroethoxy)benzoic Acid

生成物 1

HCID 2727094Methyl 2,5-bis(2,2,2-trifluoroethoxy)benzoate収率 98%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2,5-bis(2,2,2-trifluoroethoxy)benzoic acid (20 g) and thionyl chloride (15.0 g) in methanol (100 ml) was stirred at 80° C. for 2 hours. The solvents were evaporated under vacuum to give an oil residue. Toluene (100 ml) was added to the residue and the solution was washed with saturated NaHCO3 (30 ml) solution followed by water (3×30 ml). The organic layer was concentrated under reduced pressure to give the product as a white solid (20.5 g, yield 98.0%).

後処理

  1. customThe solvents were evaporated under vacuum
  2. customto give an oil residue
  3. washthe solution was washed with saturated NaHCO3 (30 ml) solution
  4. concentrationThe organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-8a2a5e9993e74072941f4e4b4d260e81
出典データセット
uspto-grants-2007_03
特許番号
US07196197B2

関連ノート

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