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Triethylamine → o-Methoxycarbonyl--[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide

HRID 1381190
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Reaktionsgleichung

Reaktionsgleichung von HRID 1381190
[CH3:1][O:2][C:3]([C:5]1[CH:20]=[CH:19][CH:18]=[CH:17][C:6]=1[NH:7][C:8](=[O:16])[CH2:9][N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)=[O:4].C(N(CC)CC)C.[CH3:28][O:29][C:30]1[CH:31]=[C:32]([CH:36]=[CH:37][C:38]=1[O:39][CH3:40])[C:33](Cl)=[O:34]>C(Cl)Cl>[CH3:1][O:2][C:3]([C:5]1[CH:20]=[CH:19][CH:18]=[CH:17][C:6]=1[NH:7][C:8](=[O:16])[CH2:9][N:10]1[CH2:15][CH2:14][N:13]([C:33](=[O:34])[C:32]2[CH:36]=[CH:37][C:38]([O:39][CH3:40])=[C:30]([O:29][CH3:28])[CH:31]=2)[CH2:12][CH2:11]1)=[O:4]
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Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 77070Veratroyl chlorideHCID 13117362o-Methoxycarbonyl-alpha-(1-piperazinyl)acetanilide

Produkt 1

HCID 13117363o-Methoxycarbonyl--[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]acetanilide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

6.5 Grams of o-methoxycarbonyl-α-(1-piperazinyl)acetanilide and 2.4 g of triethylamine were dissolved in 50 ml of methylene chloride, then a methylene chloride solution containing 5.4 g of 3,4-dimethoxybenzoyl chloride was added dropwise thereto under ice-cooled condition with stirring. The reaction was continued at the same temperature for 1 hour, then the reaction mixture was washed with water, 5%-sodium bicarbonate aqueous solution, next with potassium carbonate aqueous solution, and was dried. Methylene chloride was removed by distillation, the residue obtained was crystallized by adding ethyl acetate, the crystals formed were collected by filtration. Recrystallized from ethanol to obtain 7.5 g of o-methoxycarbonyl-α-[4-(3,4-dimethoxy-benzoyl)-1-piperazinyl]acetanilide in the form of colorless needle-like crystals. Melting point: 167.5°-169° C.

Aufarbeitung

  1. additionwas added dropwise
  2. temperatureunder ice-cooled condition
  3. washthe reaction mixture was washed with water, 5%-sodium bicarbonate aqueous solution, next with potassium carbonate aqueous solution
  4. customwas dried
  5. customMethylene chloride was removed by distillation
  6. customthe residue obtained
  7. customwas crystallized
  8. additionby adding ethyl acetate
  9. customthe crystals formed
  10. filtrationwere collected by filtration
  11. customRecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-7fd697e16f894d51828b886afb75e08b
Quelldatensatz
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04585774

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