Water → N'-(3-cyano-5-iodopyrazin-2-yl)-N,N-dimethylformimidamide

HRID 334385노트

반응식

HRID 334385 반응식
P(Cl)(Cl)(Cl)=O.[NH2:6][C:7]1[C:8]([C:14]([NH2:16])=O)=[N:9][C:10]([I:13])=[CH:11][N:12]=1.O.[CH3:18][N:19]([CH3:22])[CH:20]=O>>[C:14]([C:8]1[C:7]([N:6]=[CH:18][N:19]([CH3:22])[CH3:20])=[N:12][CH:11]=[C:10]([I:13])[N:9]=1)#[N:16]

참가 물질

5

반응물 4

HCID 962WaterHCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 468639523-Amino-6-iodopyrazine-2-carboxamide

생성물 1

HCID 86680553N'-(3-cyano-5-iodopyrazin-2-yl)-N,N-dimethylformimidamide수율 84%

실험 절차

13.59 ml (146 mmol) of phosphorus oxychloride is added drop by drop at 0° C. to 11 g (41.7 mmol) of a solution of 3-amino-6-iodopyrazine-2-carboxamide in 80 ml of dimethylformamide. The reaction mixture is stirred at room temperature overnight and then poured in a beaker containing ice and a little water. The pH is adjusted to 8 with 1 N soda solution; a precipitate is formed. The mixture is allowed to gradually return to room temperature and then the solid formed is filtered, rinsed with water and dried at 50° C. to yield 10.50 g of N′-(3-cyano-5-iodopyrazine-2-yl)-N,N-dimethyl formimidamide (84%) in the form of a beige solid.

후처리

  1. additionpoured in a beaker
  2. additioncontaining ice
  3. customa precipitate is formed
  4. customto gradually return to room temperature
  5. customthe solid formed
  6. filtrationis filtered
  7. washrinsed with water
  8. customdried at 50° C.

출처 및 근거

ORD 기록
ord-8e059d6ea9a041a5b2e2fb4d7888fcb8
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883821B2

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