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Acetonitrile → o-Carbamoyl-alpha-(4-benzyl-1-piperazinyl)acetanilide dihydrochloride

HRID 1381188
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1381188
[C:1]([C:4]1[CH:14]=[CH:13][CH:12]=[CH:11][C:5]=1[NH:6][C:7](=[O:10])[CH2:8][Cl:9])(=[O:3])[NH2:2].[CH2:15]([N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(N(CC)CC)C.C(#N)C>C(O)C>[ClH:9].[ClH:9].[C:1]([C:4]1[CH:14]=[CH:13][CH:12]=[CH:11][C:5]=1[NH:6][C:7](=[O:10])[CH2:8][N:25]1[CH2:26][CH2:27][N:22]([CH2:15][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:23][CH2:24]1)(=[O:3])[NH2:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 6342AcetonitrileHCID 8471TriethylamineHCID 759941-BenzylpiperazineHCID 5198892'-Carbamoyl-2-chloroacetanilide

Produkt 1

HCID 23323546o-Carbamoyl-alpha-(4-benzyl-1-piperazinyl)acetanilide dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702
Ethanol
Lösungsmittel

Versuchsvorschrift

40 Grams of o-carbamoyl-α-chloroacetanilide, 40 g of benzylpiperazine, 52.4 ml of triethylamine and 250 ml of acetonitrile were heated at 50° C. for 5 hours with stirring, and crystals formed were collected by filtration. The crystals collected were extracted with chloroform and 1 N-sodium hydroxide aqueous solution, the chloroform layer was washed with water, dried then chloroform was removed by distillation. To the residue obtained was added ethanol and insoluble material formed was collected by filtration. Then the insoluble material was suspended in ethanol and was added hydrochloric acid/ethanol to make the pH of the mixture to about 1, then the solvent was removed by distillation. The residue obtained was crystallized by adding acetone, and recrystallized from methanol to obtain 54 g of o-carbamoyl-α-(4-benzyl-1-piperazinyl)acetanilide dihydrochloride. Colorless powdery crystals. Melting point: 218.5°-219.5° C. (decomposed).

Aufarbeitung

  1. customcrystals formed
  2. filtrationwere collected by filtration
  3. customThe crystals collected
  4. extractionwere extracted with chloroform and 1 N-sodium hydroxide aqueous solution
  5. washthe chloroform layer was washed with water
  6. customdried
  7. customchloroform was removed by distillation
  8. customTo the residue obtained
  9. customformed
  10. filtrationwas collected by filtration
  11. additionwas added hydrochloric acid/ethanol
  12. customthe solvent was removed by distillation
  13. customThe residue obtained
  14. customwas crystallized
  15. additionby adding acetone
  16. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-598854da5a1849c4aa26e9017d64ff48
Quelldatensatz
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04585774

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