Dimethylformamide → HCID 86646773, 화합물

HRID 913280노트

반응식

HRID 913280 반응식
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

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6344DichloromethaneHCID 24813Phosphorus oxychlorideHCID 178512299HCID 178512299, 화합물2회

생성물 1

HCID 86646773HCID 86646773, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-2756d7f1cc684dfc8ad3a127d1c7d536
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026359B2

반응 노트

불러오는 중…