2,2,2-Trifluoroethanol → 4-(4-(2,6-dimethyl-4-(pyridin-4-yl)phenoxy)-1H-pyrazolo[3,4-d]pyrimidin-6-ylamino)benzonitrile

反応式

F[C:2](F)(F)C(O)=O.[CH3:8][C:9]1[CH:25]=[C:24]([C:26]2[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=2)[CH:23]=[C:22]([CH3:32])[C:10]=1[O:11][C:12]1[C:13]2N[N:20]=[N:19][C:14]=2[N:15]=[C:16](Cl)[N:17]=1.[NH2:33][C:34]1[CH:41]=[CH:40][C:37]([C:38]#[N:39])=[CH:36][CH:35]=1.FC(F)(F)CO>>[CH3:8][C:9]1[CH:25]=[C:24]([C:26]2[CH:27]=[CH:28][N:29]=[CH:30][CH:31]=2)[CH:23]=[C:22]([CH3:32])[C:10]=1[O:11][C:12]1[N:17]=[C:16]([NH:33][C:34]2[CH:41]=[CH:40][C:37]([C:38]#[N:39])=[CH:36][CH:35]=2)[N:15]=[C:14]2[NH:19][N:20]=[CH:2][C:13]=12

参加物

反応物 4

HCID 64092,2,2-Trifluoroethanol

HCID 6422Trifluoroacetic acid

HCID 133964-Aminobenzonitrile

HCID 178422825HCID 178422825、化合物

生成物 1

HCID 441239894-(4-(2,6-dimethyl-4-(pyridin-4-yl)phenoxy)-1H-pyrazolo[3,4-d]pyrimidin-6-ylamino)benzonitrile

反応条件

温度: 90 °C

実験手順

Trifluoroacetic acid (8 eq) is added to a suspension of 7-(2,6-dimethyl-4-(pyridin-4-yl)phenoxy)-5-chloro-1H-[1,2,3]triazolo[4,5-d]pyrimidine (1 eq) and 4-aminobenzonitrile (4 eq) in 2,2,2-trifluoroethanol (1 ml/0.1 mmol) in a sealed tube. The resulting mixture is heated at 90° C. for 3 days. The reaction is cooled to room temperature, concentrated to dryness and purified by silica gel chromatography.

後処理

temperatureThe reaction is cooled to room temperature
concentrationconcentrated to dryness
custompurified by silica gel chromatography

出典と根拠

ORDレコード: ord-6f5a18608c6e494c95a1b72620d8c01c
出典データセット: uspto-grants-2013_02
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08372852B2

反応ノート

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