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

HRID 591229ノート

反応式

HRID 591229 の反応式
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]

参加物

5

反応物 3

HCID 222AmmoniaHCID 7178284-Amino-2,6-difluorobenzotrifluorideHCID 105128437-Chloro-5-methyl-2-(methylthio)-[1,2,4]triazolo[1,5-a]pyrimidine2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6df995cc0c894d5f9b02c201b225b9a2
出典データセット
uspto-grants-2016_01
特許番号
US09238653B2

反応ノート

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