Ammonia → 2-(1,1-Difluoroethyl)-5-Methyl-N-[4-(Trifluoromethyl)phenyl][1,2,4]triazolo[1,5-A]pyrimidin-7-Amine

HRID 591249노트

반응식

HRID 591249 반응식
Cl[C:2]1[N:7]2[N:8]=[C:9]([C:11]([F:14])([F:13])[CH3:12])[N:10]=[C:6]2[N:5]=[C:4]([CH3:15])[CH:3]=1.[F:16][C:17]([F:26])([F:25])[C:18]1[CH:24]=[CH:23][C:21]([NH2:22])=[CH:20][CH:19]=1.N.CO>C(O)C>[F:13][C:11]([C:9]1[N:10]=[C:6]2[N:5]=[C:4]([CH3:15])[CH:3]=[C:2]([NH:22][C:21]3[CH:23]=[CH:24][C:18]([C:17]([F:16])([F:25])[F:26])=[CH:19][CH:20]=3)[N:7]2[N:8]=1)([F:14])[CH3:12]

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 887MethanolHCID 99644-(Trifluoromethyl)anilineHCID 533918697-Chloro-2-(1,1-difluoroethyl)-5-methyl-[1,2,4]triazolo[1,5-a]pyrimidine

생성물 1

HCID 513492762-(1,1-Difluoroethyl)-5-Methyl-N-[4-(Trifluoromethyl)phenyl][1,2,4]triazolo[1,5-A]pyrimidin-7-Amine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of Intermediate 3 (10 g, 43 mmol) in ethanol (150 mL), 4-(trifluoromethyl)aniline (ALDRICH, 6.93 g, 43 mmol) was added and the mixture was stirred at room temperature for 1 h. 7M Ammonia in MeOH (6.14 mL, 43 mmol) was added to neutralize the hydrochloride salt and solvent was removed in vacuo. The crude mixture was purified by flash chromatography (Si, eluting with Hexane/EtOAc mixtures from 95:5 to 40:60%) to yield the title compound as a yellow solid.

후처리

  1. additionwas added
  2. customwas removed in vacuo
  3. customThe crude mixture was purified by flash chromatography (Si, eluting with Hexane/EtOAc mixtures from 95:5 to 40:60%)

출처 및 근거

ORD 기록
ord-24085c760348451585cc2efb4b8695b9
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238653B2

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