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

HRID 2284639
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반응식

HRID 2284639 반응식
[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
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참가 물질

6

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 962Water용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-515f098fd9e2459587ccf07c0bb9af20
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09145415B2

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