N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamine → N-[(6-chloropyridin-3-yl)methyl]-N-(2,2-difluoroethyl)-4-hydroxy-2-oxo-2,5-dihydrofuran-3-carboxamide

HRID 1192839

반응식

HRID 1192839 반응식
[OH:1][C:2]1[CH2:6][O:5][C:4](=[O:7])[C:3]=1[C:8]([O:10]C)=O.[Cl:12][C:13]1[N:18]=[CH:17][C:16]([CH2:19][NH:20][CH2:21][CH:22]([F:24])[F:23])=[CH:15][CH:14]=1>C(#N)CCC>[Cl:12][C:13]1[N:18]=[CH:17][C:16]([CH2:19][N:20]([CH2:21][CH:22]([F:24])[F:23])[C:8]([C:3]2[C:4](=[O:7])[O:5][CH2:6][C:2]=2[OH:1])=[O:10])=[CH:15][CH:14]=1

참가 물질

4

반응 조건

온도
65 °C

실험 절차

10 g of methyl 4-hydroxy-2-oxo-2,5-dihydrofuran-3-carboxylate are initially introduced in 111 g of butyronitrile and admixed with 5 g of N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamine. The solution is heated at 65° C. for 3 h. The solution is then extracted with 300 ml of water and then washed with 300 ml of 5% strength hydrochloric acid solution. The organic phase is dried over magnesium sulphate and the solvent is removed in vacuo. For purification, recrystallization from isopropanol is carried out.

후처리

  1. extractionThe solution is then extracted with 300 ml of water
  2. washwashed with 300 ml of 5% strength hydrochloric acid solution
  3. dry with materialThe organic phase is dried over magnesium sulphate
  4. customthe solvent is removed in vacuo
  5. customFor purification, recrystallization from isopropanol

출처 및 근거

ORD 기록
ord-33b2f7e565e44cbd870ad14183a7eeae
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680285B2

연결된 노트

불러오는 중…