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

HRID 524317노트

반응식

HRID 524317 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-887727e1f1444186b82426b5c479de09
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340522B2

반응 노트

불러오는 중…