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

HRID 591249ノート

反応式

HRID 591249 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 513492762-(1,1-Difluoroethyl)-5-Methyl-N-[4-(Trifluoromethyl)phenyl][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 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.

後処理

  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%)

出典と根拠

ORDレコード
ord-24085c760348451585cc2efb4b8695b9
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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