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

HRID 1968418ノート

反応式

HRID 1968418 の反応式
[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

参加物

4

反応物 2

HCID 222AmmoniaHCID 598224532-Chloro-1-(6-chloropyrimidin-4-yl)-1H-benzimidazole

生成物 1

HCID 598224556-(2-Chloro-benzoimidazol-1-yl)-pyrimidin-4-ylamine

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
50 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ce7c115d59364da58cd817432fa1063d
出典データセット
uspto-grants-2013_04
特許番号
US08426404B2

反応ノート

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