Hydrochloric Acid → 2-Chloro-4-(2,5-dichloroanilino)pyrimidine

HRID 347742

반응식

HRID 347742 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.[Cl:9][C:10]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:11]=1[NH2:12].Cl>C(O)CCC>[Cl:1][C:2]1[N:7]=[C:6]([NH:12][C:11]2[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:10]=2[Cl:9])[CH:5]=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 72622,5-DichloroanilineHCID 775312,4-Dichloropyrimidine

생성물 1

HCID 179811312-Chloro-4-(2,5-dichloroanilino)pyrimidine수율 20%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

2,4-Dichloropyrimidine (50 g, 0.34 mol), 2,5-dichloroaniline (54.38 g, 0.34 mol) and concentrated hydrochloric acid (cat. amount) were dissolved in n-butanol (250 ml). The reaction mixture was stirred at room temperature for 12 hours after which the solid that had formed was collected by filtration. The organics were allowed to stand for 48 hours and the solid that formed was collected by filtration, washed with EtOAc and dried to give the title product as a white solid (18.65 g). NMR (300 MHz): 6.82 (d, 1H), 7.31 (dd, 1H), 7.58 (d, 1H), 7.82 (s, 1H), 8.19 (d, 1H), 9.82 (s, 1H); m/z: (ES+) 273.9 (MH+).

후처리

  1. customthat had formed
  2. filtrationwas collected by filtration
  3. waitto stand for 48 hours
  4. customthe solid that formed
  5. filtrationwas collected by filtration
  6. washwashed with EtOAc
  7. customdried

출처 및 근거

ORD 기록
ord-44c263d9e5d5409fb10eec7b770bee1f
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176212B2

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