Ammonium Hydroxide → HCID 66984885, 화합물

HRID 1950778노트

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HRID 1950778 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:11][C:12]2[C:17]([C:18](OCC)=[O:19])=[C:16](/[CH:23]=[CH:24]/[N:25](C)C)[N:15]=[C:14]([S:28][CH3:29])[N:13]=2)[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.[NH4+].[OH-]>CCO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:11][C:12]2[C:17]3[C:18](=[O:19])[NH:25][CH:24]=[CH:23][C:16]=3[N:15]=[C:14]([S:28][CH3:29])[N:13]=2)[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 86658932HCID 86658932, 화합물

생성물 1

HCID 66984885HCID 66984885, 화합물수율 56.5%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

The crude of (E)-ethyl 4-(3,5-dimethoxyphenylamino)-6-(2-(dimethylamino)vinyl)-2-(methylthio)pyrimidine-5-carboxylate (3.16 g) was dissolved in 45 mL EtOH. To the solution was added 30% NH4OH solution (5.2 mL), the reaction mixture was stirred at 75-85° C. for 10 hours. The mixture was cooled to room temperature. The solids formed from the solution were filtered. The filtrate was condensed under reduced pressure resulting in the solid residue. The residue was recrystallized from ethyl acetate. The combined solids were dried under reduced pressure yielding light yellow solids (1.47 g). MS m/z: 344.9 (M+H)+.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. customThe solids formed from the solution
  3. filtrationwere filtered
  4. customcondensed under reduced pressure
  5. customresulting in the solid residue
  6. customThe residue was recrystallized from ethyl acetate
  7. customThe combined solids were dried under reduced pressure

출처 및 근거

ORD 기록
ord-5601a8c9ee33490b8f1a14e43a101fa6
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404677B2

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