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 893645ノート

反応式

HRID 893645 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 gasified 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-0984acbf2ac549ffbfd6af37c467deab
出典データセット
uspto-grants-1992_06
特許番号
US05126340

反応ノート

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