4-Chloroaniline → 6-Chloro-N2-(4-chlorophenyl)pyrimidine-2,4-diamine

HRID 28546

반응식

HRID 28546 반응식
Cl[C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=1>O1CCOCC1>[Cl:9][C:4]1[N:3]=[C:2]([NH:15][C:14]2[CH:16]=[CH:17][C:11]([Cl:10])=[CH:12][CH:13]=2)[N:7]=[C:6]([NH2:8])[CH:5]=1

참가 물질

4

반응물 2

HCID 78124-ChloroanilineHCID 823874-Pyrimidinamine, 2,6-dichloro-

생성물 1

HCID 860043166-Chloro-N2-(4-chlorophenyl)pyrimidine-2,4-diamine수율 42%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 2,6-dichloro-pyrimidin-4-yl-amine (0.492 g, 3.0 mmol) and 4-chloro-aniline (1.54 g, 12.0 mmol) in dioxane (25 ml) was heated under reflux for 3 hours. After cooled to room temperature, the mixture was filtered. Concentration of the filtrate under reduced pressure provided the crude product which was purified by flash chromatography on silica gel eluting with ethyl acetate-hexane (1:3) to provide 6-chloro-N*2*-(4-chloro-phenyl)-pyrimidine-2,4-diamine (0.32 g, 42% yield) as a white powder.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. filtrationthe mixture was filtered
  4. customConcentration of the filtrate under reduced pressure provided the crude product which
  5. customwas purified by flash chromatography on silica gel eluting with ethyl acetate-hexane (1:3)

출처 및 근거

ORD 기록
ord-9eb5e6401f8f42b0be4eb920452e57df
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07419984B2

연결된 노트

불러오는 중…