Dimethylformamide dimethyl acetal → HCID 53948848, 화합물

HRID 476914노트

반응식

HRID 476914 반응식
[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]

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 13296989HCID 13296989, 화합물

생성물 1

HCID 53948848HCID 53948848, 화합물수율 99.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-37c1a83c9479454b8ae0f8c0d0b09c13
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04886807

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