Lithium Hydroxide → 5-(4-Trifluoromethyl-3-pyridyl)-1,2,4-oxadiazole-3-carboxylic acid

HRID 47218

반응식

HRID 47218 반응식
C([O:3][C:4]([C:6]1[N:10]=[C:9]([C:11]2[CH:12]=[N:13][CH:14]=[CH:15][C:16]=2[C:17]([F:20])([F:19])[F:18])[O:8][N:7]=1)=[O:5])C.[OH-].[Li+]>CO.O>[F:20][C:17]([F:18])([F:19])[C:16]1[CH:15]=[CH:14][N:13]=[CH:12][C:11]=1[C:9]1[O:8][N:7]=[C:6]([C:4]([OH:5])=[O:3])[N:10]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 227440743-Ethoxycarbonyl-5-(4-trifluoromethyl-3-pyridyl)-1,2,4-oxadiazole

생성물 1

HCID 227440715-(4-Trifluoromethyl-3-pyridyl)-1,2,4-oxadiazole-3-carboxylic acid수율 96.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

15.8 g of 3-ethoxycarbonyl-5-(4-trifluoromethyl-3-pyridyl)-1,2,4-oxadiazole are initially charged in 13 ml of methanol, and, with ice-cooling at 0° C., a solution of 2.8 g of lithium hydroxide in 50 ml of water is added dropwise. The mixture is stirred at room temperature for 2 h, 20 ml of ice-water are added and the mixture is extracted with 200 ml of diethyl ether. The aqueous phase is adjused to pH=2 using dil. HCl, and the precipitated product is filtered off with suction. After drying, 13.8 g of 5-(4-trifluoromethyl-3-pyridyl)-1,2,4-oxadiazole-3-carboxylic acid are obtained as a white solid of mp. 157-159° C.

후처리

  1. extractionthe mixture is extracted with 200 ml of diethyl ether
  2. filtrationthe precipitated product is filtered off with suction
  3. customAfter drying

출처 및 근거

ORD 기록
ord-094e15cc239749888e7b516c64dbb735
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699853B2

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