Sodium Hydroxide → [4-(4-Chloro-phenyl)-pyrimidin-2-yl]-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-amine

HRID 976265

반응식

HRID 976265 반응식
[N+]([O-])(O)=O.[F:5][C:6]([F:21])([O:10][C:11]1[CH:12]=[C:13]([NH:17][C:18]([NH2:20])=[NH:19])[CH:14]=[CH:15][CH:16]=1)[CH:7]([F:9])[F:8].CN(C)[CH:24]=[CH:25][C:26]([C:28]1[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=1)=O.[OH-].[Na+]>CC(O)C>[F:5][C:6]([F:21])([O:10][C:11]1[CH:12]=[C:13]([NH:17][C:18]2[N:20]=[C:26]([C:28]3[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=3)[CH:25]=[CH:24][N:19]=2)[CH:14]=[CH:15][CH:16]=1)[CH:7]([F:8])[F:9]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 605938(2E)-1-(4-chlorophenyl)-3-(dimethylamino)prop-2-en-1-oneHCID 1785125183-(1,1,2,2-Tetrafluoroethoxy)phenylguanidine nitrate

생성물 1

HCID 19966997[4-(4-Chloro-phenyl)-pyrimidin-2-yl]-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-amine

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

539 mg (2.15 mmol) of 3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl-guanidine nitrate are added to a solution of 450 mg (2.15 mmol) of 3-dimethylamino-1-(4-chloro-phenyl)-2-propen-1-one in 5.5 ml of 2-propanol. After the addition of 94.5 mg (2.36 mmol) of sodium hydroxide, the reaction mixture is boiled under reflux for 29 h. After cooling to RT, the product is isolated by filtration and washed with 1-propanol and water. After drying at 60° under HV, N-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-4-(4-chloro-phenyl)-2-pyrimidineamine is obtained; Rf =0.45 (methylene chloride:methanol =98:2), MS: 397 (M+), m.p. 133°-135°.

후처리

  1. temperatureunder reflux for 29 h
  2. customthe product is isolated by filtration
  3. washwashed with 1-propanol and water
  4. customAfter drying at 60° under HV

출처 및 근거

ORD 기록
ord-32387682b29b476d94088b49d2225dd9
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05612340

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