Sodium Hydroxide → N-(3-chlorophenyl)-4-(2-chloropyridin-4-yl)pyrimidin-2-amine

HRID 724813

반응식

HRID 724813 반응식
[OH-].[Na+].CN(C)[CH:5]=[CH:6][C:7]([C:9]1[CH:14]=[CH:13][N:12]=[C:11]([Cl:15])[CH:10]=1)=O.[N+]([O-])(O)=O.[Cl:21][C:22]1[CH:23]=[C:24]([NH:28][C:29]([NH2:31])=[NH:30])[CH:25]=[CH:26][CH:27]=1>CC(O)C>[Cl:21][C:22]1[CH:23]=[C:24]([NH:28][C:29]2[N:31]=[C:7]([C:9]3[CH:14]=[CH:13][N:12]=[C:11]([Cl:15])[CH:10]=3)[CH:6]=[CH:5][N:30]=2)[CH:25]=[CH:26][CH:27]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 544350393-Dimethylamino-1-(2-chloro4-pyridyl)-2-propen-1-oneHCID 178512489HCID 178512489, 화합물

생성물 1

HCID 9905031N-(3-chlorophenyl)-4-(2-chloropyridin-4-yl)pyrimidin-2-amine

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

31 mg (0.78 mmol) of sodium hydroxide are added to a suspension of 150 mg (0.7 mmol) of 3-dimethylamino-1-(2-chloro-4-pyridyl)-2-propen-1-one and 165 mg (0.71 mmol) of 3-chloro-phenyl-guanidine nitrate in 1.5 ml of 2-propanol. After stirring under reflux for 18 hours, the reaction mixture is cooled and filtered and the material retained on the filter is washed thoroughly with water. After drying (60°, HV), N-(3-chloro-phenyl)-4-(2-chloro-4-pyridyl)-2-pyrimidineamine is obtained; m.p. 196°-198°, Rf =0.67 (methylene chloride:methanol=95:5), FAB-MS: 317 (M+ +1).

후처리

  1. temperatureunder reflux for 18 hours
  2. temperaturethe reaction mixture is cooled
  3. filtrationfiltered
  4. washis washed thoroughly with water
  5. customAfter drying (60°, HV)

출처 및 근거

ORD 기록
ord-c0958cebf33340d99be644cf4c874ac8
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705502

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