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Chloroform → N-(3-(methylamino)phenyl)-4-(propylamino)-2-((2-(pyridin-4-yl)ethyl)amino)pyrimidine-5-carboxamide

HRID 2284639
ノート
印刷プレビュー

反応式

HRID 2284639 の反応式
[CH2:1]([NH:4][C:5]1[C:10]([C:11]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N:20](C)[C:21](=O)C(F)(F)F)[CH:15]=2)=[O:12])=[CH:9][N:8]=[C:7]([NH:28][CH2:29][CH2:30][C:31]2[CH:36]=[CH:35][N:34]=[CH:33][CH:32]=2)[N:6]=1)[CH2:2][CH3:3].C(=O)([O-])[O-].[K+].[K+].C(Cl)(Cl)Cl>CO.O>[CH3:21][NH:20][C:16]1[CH:15]=[C:14]([NH:13][C:11]([C:10]2[C:5]([NH:4][CH2:1][CH2:2][CH3:3])=[N:6][C:7]([NH:28][CH2:29][CH2:30][C:31]3[CH:32]=[CH:33][N:34]=[CH:35][CH:36]=3)=[N:8][CH:9]=2)=[O:12])[CH:19]=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6212ChloroformHCID 11430Potassium CarbonateHCID 900520024-(propylamino)-2-((2-(pyridin-4-yl)ethyl)amino)-N-(3-(2,2,2-trifluoro-N-methylacetamido)phenyl)pyrimidine-5-carboxamide

生成物 1

HCID 90052010N-(3-(methylamino)phenyl)-4-(propylamino)-2-((2-(pyridin-4-yl)ethyl)amino)pyrimidine-5-carboxamide収率 93.8%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 962Water溶媒2 回

実験手順

To a solution of 4-(propylamino)-2-((2-(pyridin-4-yl)ethyl)amino)-N-(3-(2,2,2 -trifluoro-N-methylacetamido)phenyl)pyrimidine-5-carboxamide (A7, 186 mg) in methanol (4 mL) and water (2 mL), potassium carbonate (92 mg) was added at room temperature, and the mixture was stirred at the same temperature for 13 hours and 30 minutes. To the reaction mixture, water and chloroform were added. The organic layer was separated, washed successively with water and saturated aqueous sodium chloride, and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain N-(3-(methylamino)phenyl)-4-(propylamino)-2-((2-(pyridin-4-yl)ethyl)amino)pyrimidine-5-carboxamide (A8, 141 mg).

後処理

  1. customThe organic layer was separated
  2. washwashed successively with water and saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-515f098fd9e2459587ccf07c0bb9af20
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09145415B2

反応ノート

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