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Sodium Hydroxide → N-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-4-(3,4,5-trimethoxyphenyl)-2-pyrimidineamine

HRID 976261
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HRID 976261 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]=[C:32]([O:34][CH3:35])[C:31]([O:36][CH3:37])=[C:30]([O:38][CH3:39])[CH:29]=1)=O.[OH-].[Na+]>C(O)CC>[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:29]=[C:30]([O:38][CH3:39])[C:31]([O:36][CH3:37])=[C:32]([O:34][CH3:35])[CH:33]=3)[CH:25]=[CH:24][N:19]=2)[CH:14]=[CH:15][CH:16]=1)[CH:7]([F:8])[F:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 539569023-(Dimethylamino)-1-(3,4,5-trimethoxyphenyl)prop-2-EN-1-oneHCID 1785125183-(1,1,2,2-Tetrafluoroethoxy)phenylguanidine nitrate

생성물 1

HCID 19966971N-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-4-(3,4,5-trimethoxyphenyl)-2-pyrimidineamine

시약·촉매·용매 1

HCID 10311-Propanol용매

실험 절차

1189.4 mg (0.75 mmol) of 3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl-guanidine nitrate are added to a solution of 200 mg (0.75 mmol) of 3-dimethylamino-1-(3,4,5-trimethoxy-phenyl)-2-propen-1-one in 11.5 ml of 1-propanol. After the addition of 33.2 mg (0.83 mmol) of sodium hydroxide, the reaction mixture is boiled under reflux for 23 hours. After cooling to RT, the reaction product is isolated by filtration and washed with 1-propanol and water. After drying at 60° C. under HV, N-[3-(1,1,2,2-tetrafluoro-ethoxy)-phenyl]-4-(3,4,5-trimethoxyphenyl)-2-pyrimidineamine is obtained; Rf =0.75 (methylene chloride:methanol=9:1), FAB-MS: 454 (M+ +1), m.p. 132° C.

후처리

  1. temperatureunder reflux for 23 hours
  2. customthe reaction product is isolated by filtration
  3. washwashed with 1-propanol and water
  4. customAfter drying at 60° C. under HV

출처 및 근거

ORD 기록
ord-0ff0197f2f604f8d969bfc55178f84ff
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05612340

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