Benzyl Chloride → 3-Dibenzylaminophenoxyacetic acid methylester

HRID 414874노트

반응식

HRID 414874 반응식
[CH3:1][O:2][C:3](=[O:13])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([NH2:12])[CH:7]=1.C(=O)([O-])[O-].[Na+].[Na+].[CH2:20](Cl)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>>[CH3:1][O:2][C:3](=[O:13])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([N:12]([CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:7]=1

참가 물질

4

반응물 3

HCID 7503Benzyl ChlorideHCID 10340Sodium CarbonateHCID 10678961Methyl 2-(3-aminophenoxy)acetate

생성물 1

HCID 866565173-Dibenzylaminophenoxyacetic acid methylester

반응 조건

온도
100 °C

실험 절차

10 g of 3-aminophenoxyacetic acid methylester are solved in 19 g benzyl chloride. Subsequently, 14 g of sodium carbonate are added portionwise and the temperature is raised to 100° C. The reaction mixture is stirred at this temperature for 3 hours. The insoluble salt is filtered off and washed with 100 ml of ethyl acetate. The combined filtrates are kept at 5° C. for 12 h. After the extraction with water and brine, the organic phase is dried with sodium sulfate and the solvent is removed in vacuum (50° C., 10−2 mbar). Yield: 22 g (dark oil).

후처리

  1. filtrationThe insoluble salt is filtered off
  2. washwashed with 100 ml of ethyl acetate
  3. waitThe combined filtrates are kept at 5° C. for 12 h
  4. extractionAfter the extraction with water and brine
  5. dry with materialthe organic phase is dried with sodium sulfate
  6. customthe solvent is removed in vacuum (50° C., 10−2 mbar)

출처 및 근거

ORD 기록
ord-d8f41782269540beb5e0c23e78fbed88
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088182B2

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