Anthranilamide → Benzamide, 2-((2-(4-(2-phenylethyl)-1-piperazinyl)ethyl)amino)-, monohydrochloride

HRID 1439599ノート

反応式

HRID 1439599 の反応式
[C:1]([NH2:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[NH2:4].Cl.Cl.[CH2:13]([N:21]1[CH2:26][CH2:25][N:24]([CH2:27][CH2:28][Cl:29])[CH2:23][CH2:22]1)[CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C([O-])(=O)C.[Na+].[NH4+].[OH-]>O>[ClH:29].[CH2:13]([N:21]1[CH2:26][CH2:25][N:24]([CH2:27][CH2:28][NH:4][C:3]2[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=2[C:1]([NH2:10])=[O:9])[CH2:23][CH2:22]1)[CH2:14][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

6

反応物 4

HCID 6942AnthranilamideHCID 14923Ammonium HydroxideHCID 517045Sodium AcetateHCID 70587748HCID 70587748、化合物

生成物 1

HCID 3050159Benzamide, 2-((2-(4-(2-phenylethyl)-1-piperazinyl)ethyl)amino)-, monohydrochloride収率 23.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of 13.6 g anthranilamide, 34.5 g 4-phenethylpiperazinoethyl chloride dihydrochloride, 17.5 g sodium acetate, and 50 ml water was refluxed for 24 hours, 50 ml water and 50 m/NH4OH was added and the mixture cooled. The liquid was decanted and the oily solid dissolved in 100 ml propanol, 200 ml water added and the solid filtered. The solid was dissolved in 2 liters of dry ether, acidified with dry HCl gas and filtered. The HCl salt was recrystallized from propanol to give 9.2 g product.

後処理

  1. temperaturewas refluxed for 24 hours
  2. temperaturethe mixture cooled
  3. customThe liquid was decanted
  4. dissolutionthe oily solid dissolved in 100 ml propanol
  5. addition200 ml water added
  6. filtrationthe solid filtered
  7. dissolutionThe solid was dissolved in 2 liters of dry ether
  8. filtrationfiltered
  9. customThe HCl salt was recrystallized from propanol

出典と根拠

ORDレコード
ord-24d4020c9cdf41c4860bca713d8c1024
出典データセット
uspto-grants-1977_11
特許番号
US04060526

反応ノート

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