Potassium Carbonate → HCID 86725664、化合物

HRID 514558

反応式

HRID 514558 の反応式
CS(O[CH2:6][CH2:7][C:8]1[CH:9]=[N:10][N:11]([C:13]2[CH:18]=[C:17]([C:19]#[N:20])[CH:16]=[CH:15][N:14]=2)[CH:12]=1)(=O)=O.[F:21][C:22]1[CH:30]=[CH:29][C:25]([CH2:26][NH:27][CH3:28])=[CH:24][CH:23]=1.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[F:21][C:22]1[CH:30]=[CH:29][C:25]([CH2:26][N:27]([CH3:28])[CH2:6][CH2:7][C:8]2[CH:9]=[N:10][N:11]([C:13]3[CH:18]=[C:17]([C:19]#[N:20])[CH:16]=[CH:15][N:14]=3)[CH:12]=2)=[CH:24][CH:23]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 7368601-(4-fluorophenyl)-N-methylmethanamineHCID 86725665HCID 86725665、化合物

生成物 1

HCID 86725664HCID 86725664、化合物収率 50.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

To a mixture of 2-[1-(4-cyanopyridin-2-yl)pyrazol-4-yl]ethyl methanesulfonate (476 mg, 1.6 mmol) and (4-flouro-benzyl)-methyl-amine (444 mg, 3.2 mmol) in ACN (30 mL) at rt was added K2CO3 (4.5 g, 32 mmol) and KI (1.0 g, 6.2 mmol. The reaction mixture was heated to 80° C. and stirred overnight. Filtered, solvent removed and purified by prep-HPLC to give the title compound (270 mg, 50%). [M+H] Calc'd for C19H18FN5, 336. Found, 336.

後処理

  1. filtrationFiltered
  2. customsolvent removed
  3. custompurified by prep-HPLC

出典と根拠

ORDレコード
ord-86447b2a9d744996b4ac6bc4175d3280
出典データセット
uspto-grants-2015_08
特許番号
US09107916B2

関連ノート

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