Water → Benzyl 5-(benzyloxy)-2-methylbenzoate

HRID 524317ノート

反応式

HRID 524317 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:11])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].C(=O)([O-])[O-].[K+].[K+].[CH2:18](Cl)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.O>CN(C=O)C.CC(=O)OCC>[CH2:18]([O:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:11])=[C:6]([CH:10]=1)[C:7]([O:9][CH2:11][C:5]1[CH:6]=[CH:10][CH:2]=[CH:3][CH:4]=1)=[O:8])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

参加物

7

反応物 4

HCID 962WaterHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 2351885-Hydroxy-2-methylbenzoic acid

生成物 1

HCID 67363220Benzyl 5-(benzyloxy)-2-methylbenzoate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

A mixture of 2.6 g of 5-hydroxy-2-methylbenzoic acid (see below), 7.0 g potassium carbonate and 3.8 ml benzyl chloride in 50 ml DMF are stirred at 50° C. for two hours, until the reaction is completed according to TLC analysis. The reaction mixture is portioned between water and EA, and the phases are separated. The organic phase is washed three times with 1 M sodium carbonate solution and once with brine, dried over MgSO4, and the solvent is removed under reduced pressure yielding benzyl 5-(benzyloxy)-2-methylbenzoate, which is used for the next step without further purification.

後処理

  1. customthe phases are separated
  2. washThe organic phase is washed three times with 1 M sodium carbonate solution
  3. dry with materialonce with brine, dried over MgSO4
  4. customthe solvent is removed under reduced pressure

出典と根拠

ORDレコード
ord-887727e1f1444186b82426b5c479de09
出典データセット
uspto-grants-2016_05
特許番号
US09340522B2

反応ノート

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