Hydrochloric Acid → 1-Chlorocarbonyl-4-piperidinopiperidine hydrochloride

HRID 1444681

Reaktionsgleichung

Reaktionsgleichung von HRID 1444681
[N:1]1([CH:7]2[CH2:12][CH2:11][N:10]([C:13]([Cl:15])=[O:14])[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.CCC1C2CN3C(=O)C4COC([C@](O)(CC)C=4C=C3C=2N=C2C=1C=C(OC(N1CCC(N3CCCCC3)CC1)=O)C=C2)=O.N1(C2CCNCC2)CCCCC1.C(Cl)(Cl)=O>C(Cl)Cl>[ClH:15].[N:1]1([CH:7]2[CH2:8][CH2:9][N:10]([C:13]([Cl:15])=[O:14])[CH2:11][CH2:12]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Komponenten

7

Edukt 5

HCID 313Hydrochloric AcidHCID 6371PhosgeneHCID 60838IrinotecanHCID 786071,4'-BipiperidineHCID 98133754-Piperidinopiperidine-1-carbonyl chloride

Produkt 1

HCID 116375531-Chlorocarbonyl-4-piperidinopiperidine hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

The present invention is related to a process for the preparation of [1,4′]bipiperidinyl-1′-carbonyl chloride or its hydrochloride, which is a useful intermediate e.g. in the preparation of irinotecan. The use of methylene chloride as a solvent in the reaction of 4-piperidinopiperidine with phosgene and the removal of the reaction solvent by using an additional distillation solvent to raise the distillation temperature gives [1,4′]bipiperidinyl-1′-carbonyl chloride hydrochloride in high yield and purity. The amount of dimer impurity will be less than 5%, even less than 1%.

Aufarbeitung

  1. customthe removal of the reaction solvent
  2. temperatureto raise the distillation temperature

Quellen und Nachweise

ORD-Eintrag
ord-307a945911784462bcfbc42f9d5d1eb0
Quelldatensatz
uspto-grants-2010_02
Patentnummer
US07662964B2

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