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Sodium Hydroxide → 2-Amino-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]cinnamic acid

HRID 1649201
ノート
印刷プレビュー

反応式

HRID 1649201 の反応式
[N+:1]([C:4]1[CH:14]=[CH:13][C:12]([N:15]2[CH2:20][CH2:19][N:18]([C:21](=[O:32])[C:22]3[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH3:31])[CH:23]=3)[CH2:17][CH2:16]2)=[CH:11][C:5]=1[CH:6]=[CH:7][C:8]([OH:10])=[O:9])([O-])=O.[OH-].[Na+]>Cl.CO>[NH2:1][C:4]1[CH:14]=[CH:13][C:12]([N:15]2[CH2:16][CH2:17][N:18]([C:21](=[O:32])[C:22]3[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH3:31])[CH:23]=3)[CH2:19][CH2:20]2)=[CH:11][C:5]=1[CH:6]=[CH:7][C:8]([OH:10])=[O:9]
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 2

HCID 14798Sodium HydroxideHCID 543143522-Nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]cinnamic acid

生成物 1

HCID 542573532-Amino-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]cinnamic acid収率 56.3%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒2 回HCID 887Methanol溶媒

実験手順

2-Nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]cinnamic acid (12 g) was dissolved in 60 ml of concentrated hydrochloric acid and to the resulting solution was added dropwise a solution of 20 g of stannous chloride in 40 ml of concentrated hydrochloric acid at room temperature. After stirring for 2 hours crystals which precipitated were collected by filtration. The crystals thus-obtained was dissolved in 240 ml of methanol and the solution was neutralized with 10% aqueous sodium hydroxide solution to precipitate crystals, which then were collected by filtration. After concentrating the methanol solution, the residue was recrystallized from ethanol to give 6.3 g of 2-amino-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]cinnamic acid, m.p. 168°-170.5° C., pale yellow powders.

後処理

  1. customprecipitated
  2. filtrationwere collected by filtration
  3. customThe crystals thus-obtained
  4. customto precipitate crystals, which
  5. filtrationthen were collected by filtration
  6. concentrationAfter concentrating the methanol solution
  7. customthe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-084f2b142f5a4ebe8365d579999e9838
出典データセット
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04415572

反応ノート

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