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

HRID 1439599노트

반응식

HRID 1439599 반응식
[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

참가 물질

6

반응물 4

HCID 6942AnthranilamideHCID 14923Ammonium HydroxideHCID 517045Sodium AcetateHCID 70587748HCID 70587748, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-24d4020c9cdf41c4860bca713d8c1024
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04060526

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