Dimethylformamide → HCID 86646773、化合物

HRID 913280ノート

反応式

HRID 913280 の反応式
CN(C)C=O.P(Cl)(Cl)(Cl)=O.[Cl:11][C:12]1[N:17]=[C:16]([C:18](=[NH:22])[NH:19][C:20]#[N:21])[CH:15]=[CH:14][N:13]=1.[CH2:23](Cl)[Cl:24]>C(#N)C>[Cl:24][C:23]1[N:22]=[C:18]([C:16]2[CH:15]=[CH:14][N:13]=[C:12]([Cl:11])[N:17]=2)[N:19]=[CH:20][N:21]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6344DichloromethaneHCID 24813Phosphorus oxychlorideHCID 178512299HCID 178512299、化合物2 回

生成物 1

HCID 86646773HCID 86646773、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To an ice-cooled solution of N,N-dimethylformamide (8.5 mL, 110 mmol) in methylene chloride (100 mL) was added phosphorus oxychloride (8.0 mL, 87 mmol) dropwise, and the mixture was stirred for 0.5 h. The resulting mixture was poured into a cold (0° C.) suspension of 2-chloro-N-cyano-4-pyrimidinecarboximidamide (i.e., the product of Step A) (13 g, 73 mmol) in acetonitrile (200 mL). The resulting mixture was stirred overnight in an ice bath. The mixture was passed through a short silica gel pad, eluted with 30% ethyl acetate in hexanes, and concentrated under reduced pressure to give 7 g of the title compound as a white solid.

後処理

  1. stirringThe resulting mixture was stirred overnight in an ice bath
  2. washeluted with 30% ethyl acetate in hexanes
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2756d7f1cc684dfc8ad3a127d1c7d536
出典データセット
uspto-grants-2011_09
特許番号
US08026359B2

反応ノート

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