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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
ノート
印刷プレビュー

反応式

HRID 2106571 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 79040Ethyl 2-bromopropionateHCID 5360545SodiumHCID 178517993HCID 178517993、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-51bd434a4856482c822ae67587a037dd
出典データセット
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04931083

反応ノート

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