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Ethyl chloroformate → HCID 21388470, Verbindung

HRID 1657782
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1657782
C(C(N1CCNCC1)C1C=CC([Cl:10])=CC=1)#N.C(=O)([O-])[O-].[K+].[K+].ClC(OCC)=O.[C:29]([CH:31]([N:39]1[CH2:44][CH2:43][N:42]([C:45]([O:47][CH2:48][CH3:49])=[O:46])[CH2:41][CH2:40]1)[C:32]1[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][CH:33]=1)#[N:30]>C1C=CC=CC=1.O>[ClH:10].[C:29]([CH:31]([N:39]1[CH2:44][CH2:43][N:42]([C:45]([O:47][CH2:48][CH3:49])=[O:46])[CH2:41][CH2:40]1)[C:32]1[CH:33]=[CH:34][C:35]([Cl:38])=[CH:36][CH:37]=1)#[N:30]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 10928Ethyl chloroformateHCID 11430Potassium CarbonateHCID 21388465α-(4-Chlorophenyl)-1-piperazineacetonitrileHCID 21388468HCID 21388468, Verbindung

Produkt 1

HCID 21388470HCID 21388470, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 241
Benzene
Lösungsmittel
3×
HCID 962WaterLösungsmittel

Versuchsvorschrift

To 11.7 g. of N-(α-cyano-4-chlorobenzyl)piperazine was added 70 ml. of benzene and then 6.9 g. of anhydrous potassium carbonate. To the resulting solution was added dropwise 5.4 g. of ethyl chloroformate dissolved in 30 ml. of benzene with cooling. After dropping, the mixture was stirred for 2 hours at 40° - 45°C. After cooling, water was poured into the mixture to dissolve inorganic substance. The benzene layer was separated, washed with water, dried over sodium sulfate, and the solvent distilled off. There was obtained 10.7 g. of N-(α-cyano-4-chlorobenzyl)-N'-ethoxycarbonylpiperazine as an oily substance. This product was dissolved in benzene and the resultant solution was saturated with dry hydrochloric gas to separate crystal which was collected by filtration. Recrystallization from acetone afforded N-(α-cyano-4-chlorobenzyl)-N'-ethoxycarbonylpiperazine hydrochloride having a melting point of 166°C.

Aufarbeitung

  1. additionTo the resulting solution was added dropwise 5.4 g
  2. temperatureAfter cooling
  3. dissolutionto dissolve inorganic substance
  4. customThe benzene layer was separated
  5. washwashed with water
  6. dry with materialdried over sodium sulfate
  7. distillationthe solvent distilled off
  8. customThere was obtained 10.7 g
  9. customwith dry hydrochloric gas
  10. customto separate crystal which
  11. filtrationwas collected by filtration
  12. customRecrystallization from acetone

Quellen und Nachweise

ORD-Eintrag
ord-5c62f18cb82d4f0f9db43bec1d5e405a
Quelldatensatz
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03962247

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