Potassium Carbonate → HCID 15953284、化合物

HRID 271446ノート

反応式

HRID 271446 の反応式
[NH2:1][C:2]1[N:7]2[C:8](=[O:11])[NH:9][N:10]=[C:6]2[C:5]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=2)=[C:4]([C:19]2[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=2)[N:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:33][C:34]1[CH:35]=[CH:36][C:37]([C:40]([F:43])([F:42])[F:41])=[N:38][CH:39]=1>CN(C=O)C>[NH2:1][C:2]1[N:7]2[C:8](=[O:11])[N:9]([CH2:33][C:34]3[CH:39]=[N:38][C:37]([C:40]([F:43])([F:41])[F:42])=[CH:36][CH:35]=3)[N:10]=[C:6]2[C:5]([C:12]2[CH:13]=[CH:14][C:15]([Cl:18])=[CH:16][CH:17]=2)=[C:4]([C:19]2[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=2)[N:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 27738105-(Chloromethyl)-2-(trifluoromethyl)pyridineHCID 58772836HCID 58772836、化合物

生成物 1

HCID 15953284HCID 15953284、化合物収率 67.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

To a mixture of crude 5-amino-7,8-bis(4-chlorophenyl)-[1,2,4]triazolo[4,3-c]pyrimidin-3(2H)-one (26 mg, 0.07 mmol), DMF (0.5 mL), and potassium carbonate (45 mg, 0.32 mmol) was added 5-chloromethyl-2-(trifluoromethyl)pyridine (21.2 mg, 0.11 mmol). The resulting reaction mixture was stirred at 50° C. for 80 min. The reaction mixture was purified by preparative reverse phase HPLC without prior workup to obtain 25 mg of the title compound as a light yellow solid. HPLC/MS: retention time=4.14 min, [M+H]30 =531.

後処理

  1. customThe resulting reaction mixture
  2. customThe reaction mixture was purified by preparative reverse phase HPLC without prior workup

出典と根拠

ORDレコード
ord-159433babcd8424b83aac50df788486c
出典データセット
uspto-grants-2008_11
特許番号
US07452892B2

反応ノート

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