1-(2-Pyridyl)piperazine → 4,5-Dihydro-6-methyl-4-[[4-(2-pyridinyl)-1-piperazinyl]acetyl]-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrile

HRID 1088759ノート

反応式

HRID 1088759 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1.Cl[CH2:14][C:15]([N:17]1[CH2:22][C:21]([CH3:23])=[C:20]([C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([C:30]([F:33])([F:32])[F:31])[CH:25]=2)[N:19]2[N:34]=[CH:35][C:36]([C:37]#[N:38])=[C:18]12)=[O:16]>CC(C)=O>[CH3:23][C:21]1[CH2:22][N:17]([C:15](=[O:16])[CH2:14][N:10]2[CH2:9][CH2:8][N:7]([C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=3)[CH2:12][CH2:11]2)[C:18]2[N:19]([N:34]=[CH:35][C:36]=2[C:37]#[N:38])[C:20]=1[C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([C:30]([F:31])([F:32])[F:33])[CH:25]=1

参加物

4

反応物 2

HCID 944591-(2-Pyridyl)piperazineHCID 151010854-(Chloroacetyl)-4,5-dihydro-6-methyl-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]-pyrimidine-3-carbonitrile

生成物 1

HCID 151010474,5-Dihydro-6-methyl-4-[[4-(2-pyridinyl)-1-piperazinyl]acetyl]-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrile収率 100.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 2 g of 1-(2-pyridinyl)piperazine, 2 g of 4-(chloroacetyl)-4,5-dihydro-6-methyl-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrile and 60 ml of acetone was refluxed on a steam bath for 8 hours and then evaporated. The residue was stirred in water and the solid collected. The solid was dissolved in dilute hydrochloric acid, filtered and the filtrate basified with dilute ammonium hydroxide. The solid was collected, washed with water and dried in vacuo, giving 2.67 g of the desired product, mp 132°-134° C.

後処理

  1. temperaturewas refluxed on a steam bath for 8 hours
  2. customevaporated
  3. customthe solid collected
  4. dissolutionThe solid was dissolved in dilute hydrochloric acid
  5. filtrationfiltered
  6. customThe solid was collected
  7. washwashed with water
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-390c86f84ccc49798bd6bf6f9baf5f77
出典データセット
uspto-grants-1990_10
特許番号
US04963553

反応ノート

読み込み中…