Dimethylformamide dimethyl acetal → HCID 53948848、化合物

HRID 476914ノート

反応式

HRID 476914 の反応式
[NH2:1][C:2]1[N:7]([CH3:8])[C:6](=[O:9])[N:5]([CH3:10])[C:4](=[O:11])[C:3]=1[C:12]#[N:13].CO[CH:16](OC)[N:17]([CH3:19])[CH3:18]>CN(C)C=O>[C:12]([C:3]1[C:4](=[O:11])[N:5]([CH3:10])[C:6](=[O:9])[N:7]([CH3:8])[C:2]=1[N:1]=[CH:16][N:17]([CH3:19])[CH3:18])#[N:13]

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 13296989HCID 13296989、化合物

生成物 1

HCID 53948848HCID 53948848、化合物収率 99.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3.6 g (20 mmol) of 6-amino-5-cyano-1,3-dimethyluracil and 9.36 g (80 mmol) of dimethylformamide dimethyl acetal were added to 36 ml of dimethylformamide, and the reaction mixture was refluxed for 30 minutes. The solvent was removed by distillation under reduced pressure. The crude product was crystallized from ether, filtered off, and recrystallized from ethyl acetate to give 4.68 g of 5-cyano-6-dimethylaminomethyleneamino-1,3-dimethyluracil (compound 15) in a 99% yield.

後処理

  1. temperaturethe reaction mixture was refluxed for 30 minutes
  2. customThe solvent was removed by distillation under reduced pressure
  3. customThe crude product was crystallized from ether
  4. filtrationfiltered off
  5. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-37c1a83c9479454b8ae0f8c0d0b09c13
出典データセット
uspto-grants-1989_12
特許番号
US04886807

反応ノート

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