Water → methyl N-{2-[4-(1-methylpropoxy)phenoxy]ethyl}carbamate

HRID 2309844노트

반응식

HRID 2309844 반응식
[CH3:1][CH:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)[CH2:3][CH3:4].Cl[CH2:14][CH2:15][NH:16][C:17](=[O:20])[O:18][CH3:19].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:1][CH:2]([O:5][C:6]1[CH:7]=[CH:8][C:9]([O:12][CH2:14][CH2:15][NH:16][C:17](=[O:20])[O:18][CH3:19])=[CH:10][CH:11]=1)[CH2:3][CH3:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 251614Methyl (2-chloroethyl)carbamateHCID 138820044-(1-Methyl-1-propyloxy)-phenol

생성물 1

HCID 15662569methyl N-{2-[4-(1-methylpropoxy)phenoxy]ethyl}carbamate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4-(1-methylpropoxy)phenol (9.2 mmol), methyl 2-chloroethylcarbamate (11.9 mmol), and potassium carbonate (18.4 mmol) in 20 ml of dimethylformamide (DMF) is heated at 85° for 18 hours. The reaction mixture is cooled to room temperature (RT), poured into water and extracted with ether. The combined ether extracts are washed with water until neutral, followed with brine and dried over calcium sulfate. The solvent is removed in vacuo and the residue is placed under high vacuum at 80° for ca. 2 hours to remove the excess methyl 2-chloroethylcarbamate. Purification by preparative thin layer chromatography (prep. TLC) gives methyl N-{2-[4-(1-methylpropoxy)phenoxy]ethyl}carbamate.

후처리

  1. temperatureis heated at 85° for 18 hours
  2. extractionextracted with ether
  3. washThe combined ether extracts are washed with water until neutral,
  4. dry with materialdried over calcium sulfate
  5. customThe solvent is removed in vacuo
  6. customto remove the excess methyl 2-chloroethylcarbamate
  7. customPurification by preparative thin layer chromatography (prep. TLC)

출처 및 근거

ORD 기록
ord-add4aaf646714895ab7b855a5ef88067
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04697033

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