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

HRID 1487355

反応式

HRID 1487355 の反応式
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]

参加物

5

反応物 4

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

生成物 1

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

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-c52882031b1440329a9a8f38408086a0
出典データセット
uspto-grants-2016_08
特許番号
US09428510B2

関連ノート

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