Hydrochloric Acid → 6-Chloro-N4-(4-chlorophenyl)pyrimidine-4,5-diamine

HRID 1246778

반응식

HRID 1246778 반응식
[NH2:1][C:2]1[C:3]([Cl:9])=[N:4][CH:5]=[N:6][C:7]=1Cl.[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=1.Cl>O.C(O)C>[Cl:9][C:3]1[N:4]=[CH:5][N:6]=[C:7]([NH:15][C:14]2[CH:16]=[CH:17][C:11]([Cl:10])=[CH:12][CH:13]=2)[C:2]=1[NH2:1]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 78124-ChloroanilineHCID 794345-Amino-4,6-dichloropyrimidine

생성물 1

HCID 167263116-Chloro-N4-(4-chlorophenyl)pyrimidine-4,5-diamine수율 99.8%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

5-amino-4,6-dichloropyrimidine (5.00 g, 29 mmol) and 4-chloroaniline (4.71 g, 36 mmol) were suspended in 80 ml H2O and 12 ml ethanol. Concentrated HCl (1.2 ml, 14.5 mmol) was added at room temperature followed by warming reaction to 82° C. After stirring for 19 hours the reaction was cooled to room temperature and stirred for 60 hours. The precipitate was collected on a sintered glass funnel and rinsed with water followed by hexanes. After drying under vacuum, I-(1A-1)a was obtained as an off-white solid (7.38 g, 98%): +ESI MS (M+1) 255.3; 1H NMR: (400 MHz, CD3OD): δ 7.87 (s, 1H), 7.66 (d, J=8.7 Hz, 2 H), 7.30 (d, J=8.7 Hz, 2 H).

후처리

  1. temperatureby warming
  2. customreaction to 82° C
  3. stirringstirred for 60 hours
  4. customThe precipitate was collected on a sintered glass funnel
  5. washrinsed with water
  6. customAfter drying under vacuum

출처 및 근거

ORD 기록
ord-93a9f1f639764b5b8afb51c603527d38
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129239B2

연결된 노트

불러오는 중…