Piperazine → 2-Piperazin-1-yl-quinazoline

HRID 1934801ノート

反応式

HRID 1934801 の反応式
Cl[C:2]1[N:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>C1(C)C=CC=CC=1>[N:12]1([C:2]2[N:11]=[CH:10][C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=2)[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1

参加物

4

反応物 2

HCID 4837PiperazineHCID 740542-Chloroquinazoline

生成物 1

HCID 64232662-Piperazin-1-yl-quinazoline

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of 2-chloroquinazoline (5 g) in 20 mL of toluene is added dropwise to a refluxing solution of piperazine (20 g) in 150 mL of toluene and the resultant solution refluxed for an additional 24 h. After cooling to 0° C. for 0.5 h, the solution is filtered and the filtrate extracted with 10% acetic acid. The aqueous extracts are washed with ether, basified and extracted with toluene. The toluene layer is then washed with water, dried and concentrated. Finally, the material is placed under vacuum overnight (6.8 g, m.p. 188-121° C.)

後処理

  1. filtrationthe solution is filtered
  2. extractionthe filtrate extracted with 10% acetic acid
  3. washThe aqueous extracts are washed with ether
  4. extractionextracted with toluene
  5. washThe toluene layer is then washed with water
  6. customdried
  7. concentrationconcentrated
  8. customis placed under vacuum overnight (6.8 g, m.p. 188-121° C.)

出典と根拠

ORDレコード
ord-61e7c71976ef420f8ed9b919d70b3242
出典データセット
uspto-grants-2002_05
特許番号
US06384224B2

反応ノート

読み込み中…