Ammonia → N-[3,5-difluoro-4-(trifluoromethyl)phenyl]-5-methyl-2-(methylthio) [1,2,4]triazolo[1,5-a]pyrimidin-7-amine

HRID 591229노트

반응식

HRID 591229 반응식
Cl[C:2]1[N:7]2[N:8]=[C:9]([S:11][CH3:12])[N:10]=[C:6]2[N:5]=[C:4]([CH3:13])[CH:3]=1.[NH2:14][C:15]1[CH:20]=[C:19]([F:21])[C:18]([C:22]([F:25])([F:24])[F:23])=[C:17]([F:26])[CH:16]=1.N>C(O)C>[F:21][C:19]1[CH:20]=[C:15]([NH:14][C:2]2[N:7]3[N:8]=[C:9]([S:11][CH3:12])[N:10]=[C:6]3[N:5]=[C:4]([CH3:13])[CH:3]=2)[CH:16]=[C:17]([F:26])[C:18]=1[C:22]([F:24])([F:25])[F:23]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 7178284-Amino-2,6-difluorobenzotrifluorideHCID 105128437-Chloro-5-methyl-2-(methylthio)-[1,2,4]triazolo[1,5-a]pyrimidine2회

생성물 1

HCID 67119775N-[3,5-difluoro-4-(trifluoromethyl)phenyl]-5-methyl-2-(methylthio) [1,2,4]triazolo[1,5-a]pyrimidin-7-amine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of 7-chloro-5-methyl-2-(methylthio)[1,2,4]triazolo[1,5-a]pyrimidine (Intermediate 8 (0.286 g, 1.332 mmol)) in ethanol (5 mL), 4-amino-2,6-difluorobenzotrifluoride (FLUOROCHEM, 0.263 g, 1.332 mmol) was added and the mixture was stirred at room temperature until reaching completion. Anhydrous ammonia (0.190 mL, 1.332 mmol) was added and solvent was removed in vacuo. The residue was purified by flash chromatography (Si, eluting with Hexane/EtOAc mixtures from 95:5 to 40:60%). Upon collection of the appropriate fractions, the title compound was obtained as a white solid.

후처리

  1. additionwas added
  2. customsolvent was removed in vacuo
  3. customThe residue was purified by flash chromatography (Si, eluting with Hexane/EtOAc mixtures from 95:5 to 40:60%)
  4. customUpon collection of the appropriate fractions

출처 및 근거

ORD 기록
ord-6df995cc0c894d5f9b02c201b225b9a2
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238653B2

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