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Dimethyl Sulfoxide → Propanoic acid, 2-((1-(3-(trifluoromethyl)phenyl)-1H-1,2,4-triazol-3-yl)oxy)-, ethyl ester

HRID 2106571
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HRID 2106571 반응식
[Na].CS(C)=O.[OH:6][C:7]1[N:11]=[CH:10][N:9]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)[N:8]=1.Br[CH:23]([CH3:29])[C:24]([O:26][CH2:27][CH3:28])=[O:25]>CO>[CH2:27]([O:26][C:24]([CH:23]([O:6][C:7]1[N:11]=[CH:10][N:9]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:19])[F:20])[CH:13]=2)[N:8]=1)[CH3:29])=[O:25])[CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 79040Ethyl 2-bromopropionateHCID 5360545SodiumHCID 178517993HCID 178517993, 화합물

생성물 1

HCID 184260Propanoic acid, 2-((1-(3-(trifluoromethyl)phenyl)-1H-1,2,4-triazol-3-yl)oxy)-, ethyl ester수율 84.1%

시약·촉매·용매 1

HCID 887
Methanol
용매

실험 절차

A 1.7 g portion of sodium was dissolved in 30 ml of methanol, and the solution was added to 150 ml of dimethylsulfoxide. To it was added 17 g of 3-hydroxy-1-(3-trifluoromethylphenyl)-1,2,4-1H-triazole, and the solution was heated on the steam bath for 90 minutes. To it was then added 13.4 g of ethyl 2-bromopropionate, and heating was continued for 90 minutes more. The mixture was then cooled and poured over ice-water. The solid was collected, dried and recrystallized from ethanol to obtain 20.5 g of the desired product, m.p. 100°-102°.

후처리

  1. temperaturethe solution was heated on the steam bath for 90 minutes
  2. temperatureheating
  3. temperatureThe mixture was then cooled
  4. customThe solid was collected
  5. customdried
  6. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-51bd434a4856482c822ae67587a037dd
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04931083

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