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Hydrogen chloride-ethyl acetate → phenylmethyl 1-[N-(piperazine-1-carbonyl)amino]cyclohexanecarboxylate

HRID 1953432
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1953432
CC(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]([NH:16][C:17]2([C:23]([O:25][CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[O:24])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[O:15])[CH2:10][CH2:9]1)=O)(C)C.Cl.C(OCC)(=O)C>C(OCC)(=O)C.Cl>[N:11]1([C:14]([NH:16][C:17]2([C:23]([O:25][CH2:26][C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=3)=[O:24])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)=[O:15])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 53984920phenylmethyl 1-[N-[4-(2-methyl-2-propyloxycarbonyl)piperazine-1-carbonyl]amino]cyclohexanecarboxylate

Produkt 1

HCID 23297891phenylmethyl 1-[N-(piperazine-1-carbonyl)amino]cyclohexanecarboxylateAusbeute 87,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittel
HCID 8857
Ethyl Acetate
Lösungsmittel

Versuchsvorschrift

2.5 g (5.6 mmol) of phenylmethyl 1-[N-[4-(2-methyl-2-propyloxycarbonyl) piperazine-1-carbonyl]amino]cyclohexanecarboxylate synthesized in Reference Example 8 was dissolved in ethyl acetate and 14 ml (56 mmol) of 4N hydrogenchloride-ethyl acetate solution (56 mmol) was added to the above prepared mixture under 0° C. and stirred for 3 hours at the room temperature. After completion of concentration of the reaction solution, the reaction solution was dissolved in 1N hydrochloric acid and washed with ethyl acetate. The water layer was separated out and was made into pH 9 with the addition of sodium carbonate and extracted three times with chloroform. The chloroform layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure, whereby 1.7 g of phenylmethyl 1-[N-(piperazine-1-carbonyl)amino]cyclohexanecarboxylate was obtained.

Aufarbeitung

  1. washwashed with ethyl acetate
  2. customThe water layer was separated out
  3. additionwas made into pH 9 with the addition of sodium carbonate
  4. extractionextracted three times with chloroform
  5. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-2ecc96b7780e4d0998e17af5ce964204
Quelldatensatz
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06117870

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