Hydrochloric Acid → 6-Oxo-5-phenyl-1,6-dihydropyrazine-2,3-dicarbonitrile

HRID 128378

반응식

HRID 128378 반응식
[NH2:1]/[C:2](/[C:7]#[N:8])=[C:3](\[NH2:6])/[C:4]#[N:5].[C:9]([C:17](O)=[O:18])(=O)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.Cl>>[C:4]([C:3]1[C:2]([C:7]#[N:8])=[N:1][C:17]([OH:18])=[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:6]=1)#[N:5]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 11915Phenylglyoxylic AcidHCID 2723951Diaminomaleonitrile

생성물 1

HCID 1785106496-Oxo-5-phenyl-1,6-dihydropyrazine-2,3-dicarbonitrile수율 90%

실험 절차

Diaminomaleonitrile (5.40 g; 0.05 mole) and 7.50 g (0.05 mole) of benzoylformic acid were put into 50 ml of a 2 N aqueous solution of hydrochloric acid. The mixture was stirred at 20° to 30° C. for 30 minutes, and further stirred at 70° to 80° C. for 2 hours. The mixture was then cooled to room temperature. The precipitate formed was collected by filtration, washed thrice with 40 ml of water, and dried under reduced pressure to afford 10.0 g (yield 90%) of 2,3-dicyano-5-hydroxy-6-phenylpyrazine.

후처리

  1. stirringfurther stirred at 70° to 80° C. for 2 hours
  2. customThe precipitate formed
  3. filtrationwas collected by filtration
  4. washwashed thrice with 40 ml of water
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-d8e4c1a032884a0b9e9672ca6684bfb7
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259489

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