4-Amino-2,6-difluorobenzotrifluoride → 2-(1,1-difluoroethyl)-N-[3,5-difluoro-4-(trifluoromethyl)phenyl]-5-methyl[1,2,4]triazolo[1,5-a]pyrimidin-7-amine

HRID 591251노트

반응식

HRID 591251 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.[NH2:16][C:17]1[CH:22]=[C:21]([F:23])[C:20]([C:24]([F:27])([F:26])[F:25])=[C:19]([F:28])[CH:18]=1>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:16][C:17]3[CH:18]=[C:19]([F:28])[C:20]([C:24]([F:27])([F:25])[F:26])=[C:21]([F:23])[CH:22]=3)[N:7]2[N:8]=1)([F:14])[CH3:12]

참가 물질

4

반응물 2

HCID 7178284-Amino-2,6-difluorobenzotrifluorideHCID 533918697-Chloro-2-(1,1-difluoroethyl)-5-methyl-[1,2,4]triazolo[1,5-a]pyrimidine

생성물 1

HCID 513475452-(1,1-difluoroethyl)-N-[3,5-difluoro-4-(trifluoromethyl)phenyl]-5-methyl[1,2,4]triazolo[1,5-a]pyrimidin-7-amine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of Intermediate 3 (0.1 g, 0.43 mmol) and 4-amino-2,6-difluorobenzotrifluoride (FLUOROCHEM, 0.085 g, 0.43 mmol) in ethanol (7 mL) was stirred at room temperature overnight. Solvent was removed in vacuo and the residue was taken up in DCM. The resulting solution was washed with 1N Na2CO3, then with brine and dried over anhydrous Na2SO4 to yield a yellow oil which was purified by flash chromatography (Si, eluting with Hexane/EtOAc mixtures from 100:0 to 50:50%) to afford the title compound as a pale yellow solid.

후처리

  1. customSolvent was removed in vacuo
  2. washThe resulting solution was washed with 1N Na2CO3
  3. dry with materialwith brine and dried over anhydrous Na2SO4
  4. customto yield a yellow oil which
  5. customwas purified by flash chromatography (Si, eluting with Hexane/EtOAc mixtures from 100:0 to 50:50%)

출처 및 근거

ORD 기록
ord-d551a552038945c9b137d26d791ed796
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238653B2

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