Ammonium Hydroxide → HCID 66984885、化合物

HRID 1950778ノート

反応式

HRID 1950778 の反応式
[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

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 86658932HCID 86658932、化合物

生成物 1

HCID 66984885HCID 66984885、化合物収率 56.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-5601a8c9ee33490b8f1a14e43a101fa6
出典データセット
uspto-grants-2013_03
特許番号
US08404677B2

反応ノート

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