ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Acetic Acid → 5-Methyl-7-phenyl-2-[4-(phenylmethyl)-1-piperazinyl]-pyrazolo[1,5-a]pyrimidine-3-carbonitrile

HRID 482874
ノート
印刷プレビュー

反応式

HRID 482874 の反応式
[C:1]1([C:7](=O)[CH2:8][C:9](=O)[CH3:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:13][C:14]1[C:18]([C:19]#[N:20])=[C:17]([N:21]2[CH2:26][CH2:25][N:24]([CH2:27][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[CH2:23][CH2:22]2)[NH:16][N:15]=1.C(O)(=O)C>ClCCl>[CH3:10][C:9]1[CH:8]=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:15]2[N:16]=[C:17]([N:21]3[CH2:26][CH2:25][N:24]([CH2:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[CH2:23][CH2:22]3)[C:18]([C:19]#[N:20])=[C:14]2[N:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 176Acetic AcidHCID 7166BenzoylacetoneHCID 1785104933-Amino-5-(4-benzyl-1-piperazinyl)-4-pyrazolecarbonitrile

生成物 1

HCID 135799875-Methyl-7-phenyl-2-[4-(phenylmethyl)-1-piperazinyl]-pyrazolo[1,5-a]pyrimidine-3-carbonitrile収率 74.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2.9 g (0.018 moles) of 1-phenyl-1,3-butanedione, 5.0 g (0.018 moles) of 3-amino-5-(4-phenylmethyl-1-piperazinyl)-4-pyrazolecarbonitrile (prepared as described in Example 1) and 25 ml of glacial acetic acid was refluxed for 4 hours. The reaction mixture was evaporated in vacuo and gave a thick oil. The oil was dissolved in dichloromethane and partitioned with saturated sodium bicarbonate. The organic layer was separated, dried over anhydrous sodium sulfate and passed through magnesium silicate. The solution was evaporated in vacuo and gave a yellow solid which was recrystallized from isopropanol and cyclohexane and gave 5.5 g of the desired product as a light yellow solid, mp 160°-164° C.

後処理

  1. temperaturewas refluxed for 4 hours
  2. customThe reaction mixture was evaporated in vacuo
  3. customgave a thick oil
  4. custompartitioned with saturated sodium bicarbonate
  5. customThe organic layer was separated
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solution was evaporated in vacuo
  8. customgave a yellow solid which
  9. customwas recrystallized from isopropanol and cyclohexane

出典と根拠

ORDレコード
ord-d2dbf030d2e94fa3be2b996bab2f0035
出典データセット
uspto-grants-1986_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04576943

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート