Potassium Carbonate → HCID 86725664、化合物

HRID 878714

反応式

HRID 878714 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 867256652-[1-(4-Cyanopyridin-2-yl)pyrazol-4-yl]ethyl methanesulfonate

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-fluoro-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-89e19dcb208b474e9683f7b400a39001
出典データセット
uspto-grants-2015_03
特許番号
US08987461B2

関連ノート

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