Ammonia → 6-(2-Chloro-benzoimidazol-1-yl)-pyrimidin-4-ylamine

HRID 1968418노트

반응식

HRID 1968418 반응식
[Cl:1][C:2]1[N:6]([C:7]2[CH:12]=[C:11](Cl)[N:10]=[CH:9][N:8]=2)[C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=2[N:3]=1.[NH3:18]>CC(O)C>[Cl:1][C:2]1[N:6]([C:7]2[N:8]=[CH:9][N:10]=[C:11]([NH2:18])[CH:12]=2)[C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=2[N:3]=1

참가 물질

4

반응 조건

온도
50 °C

실험 절차

A mixture of 2-Chloro-1-(6-chloro-pyrimidin-4-yl)-1H-benzoimidazole (500 mg, 1.89 mmol) and 10 mL 2 M Ammonia in 2-propanol is heated at 50° C. in a sealed tube for overnight. The reaction mixture is then cooled to room temperature, concentrated and treated with 10 mL H2O. The solid is collected by filtration and washed with water, dried to afford the title compound as a solid: 1H NMR 400 MHz (DMSO-d6) δ 8.50 (s, 1H), 7.72-7.67 (m, 1H), 7.60-7.55 (m, 1H), 7.44 (s, 2H), 7.37-7.31 (m, 2H), 6.71 (dd, J=1.2 Hz, 1H); MS m/z 246.1 (M+1).

후처리

  1. temperatureThe reaction mixture is then cooled to room temperature
  2. concentrationconcentrated
  3. additiontreated with 10 mL H2O
  4. filtrationThe solid is collected by filtration
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-ce7c115d59364da58cd817432fa1063d
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08426404B2

반응 노트

불러오는 중…