Water → Imidazo (2,1-b)-1,3,4-thiadiazole, 2-(methoxymethyl)-6-(trifluoromethyl)-

HRID 69558

반응식

HRID 69558 반응식
Br[CH2:2][C:3]([C:5]([F:8])([F:7])[F:6])=O.[CH3:9][O:10][CH2:11][C:12]1[S:16][C:15]([NH2:17])=[N:14][N:13]=1.O>COCCOC>[CH3:9][O:10][CH2:11][C:12]1[S:16][C:15]2=[N:17][C:3]([C:5]([F:8])([F:7])[F:6])=[CH:2][N:14]2[N:13]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 790083-Bromo-1,1,1-trifluoro-2-propanoneHCID 6608445-(Methoxymethyl)-1,3,4-thiadiazol-2-amine

생성물 1

HCID 67117085Imidazo (2,1-b)-1,3,4-thiadiazole, 2-(methoxymethyl)-6-(trifluoromethyl)-수율 47%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
80 °C

실험 절차

Bromotrifluoroacetone (478 g, 1.05 eq) is added on a suspension of 5-(methoxymethyl)-1,3,4-thiadiazol-2-amine a25 (346 g, 1 eq) in 1,2-dimethoxyethane (6 l) at 20° C. The reaction mixture is heated to 80° C. until maximum conversion (<24 h). Water (4 l) is added to the reaction mixture at 32° C. and the expected compound crystallized out of the reaction mixture. The crystalline suspension is cooled to 10° C. to complete the crystallization process, filtered and the crystalline precipitate is washed with water (1.5 l) to afford 266 g of pure 2-(methoxymethyl)-6-(trifluoromethyl)imidazo[2,1-b][1,3,4]thiadiazole a28.

후처리

  1. customthe expected compound crystallized out of the reaction mixture
  2. temperatureThe crystalline suspension is cooled to 10° C.
  3. filtrationfiltered
  4. washthe crystalline precipitate is washed with water (1.5 l)

출처 및 근거

ORD 기록
ord-517397c5837b4522bbf3990d126ad048
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822508B2

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