Triethylamine → 4-(3-Ethoxy-2-hydroxypropoxy)phenylcarbamoylmethyl methyl sulfide

HRID 637531노트

반응식

HRID 637531 반응식
C(N(CC)CC)C.[CH2:8]([O:10][CH2:11][CH:12]([OH:22])[CH2:13][O:14][C:15]1[CH:21]=[CH:20][C:18]([NH2:19])=[CH:17][CH:16]=1)[CH3:9].[CH3:23][S:24][CH2:25][C:26](Cl)=[O:27]>CN(C)C=O>[CH3:23][S:24][CH2:25][C:26](=[O:27])[NH:19][C:18]1[CH:17]=[CH:16][C:15]([O:14][CH2:13][CH:12]([OH:22])[CH2:11][O:10][CH2:8][CH3:9])=[CH:21][CH:20]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 107748571-(4-Aminophenoxy)-3-ethoxypropan-2-olHCID 111262562-(Methylsulfanyl)acetyl chloride

생성물 1

HCID 133860734-(3-Ethoxy-2-hydroxypropoxy)phenylcarbamoylmethyl methyl sulfide수율 95.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Dissolved in 4 ml of dimethylformamide were 2.00 g of triethylamine and 2.11 g of 4-(3-ethoxy-2-hydroxypropoxy)aniline. To the solution was added 1.25 g of methylmercaptoacetyl chloride with ice-cooling and the mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated and the residue was extracted with chloroform. The chloroform layer was washed with water and concentrated. The resulting residue was purified by silica gel column chromatography using a 1:5 ethanol-chloroform mixture, giving 2.85 g of 4-(3-ethoxy-2-hydroxypropoxy)phenylcarbamoylmethyl methyl sulfide in 95.3% yield.

후처리

  1. temperaturecooling
  2. concentrationThe reaction mixture was concentrated
  3. extractionthe residue was extracted with chloroform
  4. washThe chloroform layer was washed with water
  5. concentrationconcentrated
  6. customThe resulting residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-8a22fcf10aea48389dc7633831772e6a
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04556737

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