Reaktion #578639

ord-24b316de88374ecdbf55fa6f5cd3684c

Reaktionsgleichung

CC(C)(C)OC(=O)NNC1CCN(C(=O)OC(C)(C)C)CC1
4-(N′-tert-Butoxycarbonyl-hydrazino)-piperidine-1-carboxylic acid tert-butyl ester
CC(C)(C)OC(=O)NNC1CCN(C(=O)OC(C)(C)C)CC1
compound A6
CC(C)(C)OC(=O)NNC1CCN(C(=O)OC(C)(C)C)CC1
4-(N′-tert-Butoxycarbonyl-hydrazino)-piperidine-1-carboxylic acid tert-butyl ester
Cl
hydrochloric acid
→
Cl.Cl.NNC1CCNCC1
Piperidin-4-yl-hydrazine dihydrochloride

Edukte

CC(C)(C)OC(=O)NNC1CCN(C(=O)OC(C)(C)C)CC1
4-(N′-tert-Butoxycarbonyl-hydrazino)-piperidine-1-carboxylic acid tert-butyl ester
CC(C)(C)OC(=O)NNC1CCN(C(=O)OC(C)(C)C)CC1
compound A6
CC(C)(C)OC(=O)NNC1CCN(C(=O)OC(C)(C)C)CC1
4-(N′-tert-Butoxycarbonyl-hydrazino)-piperidine-1-carboxylic acid tert-butyl ester
Cl
hydrochloric acid

Reagenzien

Keine

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeis evaporated
  2. 2
    WaschenThe residue is washed with tetrahydrofurane
  3. 3
    Filtrationfiltered off
  4. 4
    Sonstigedried under vacuum

Vorschrift

A mixture of 0.1 mole of 4-(N′-tert-Butoxycarbonyl-hydrazino)-piperidine-1-carboxylic acid tert-butyl ester (starting compound A6) and 150 ml of concentrated hydrochloric acid is heated at 90° C. for 60 min after which the clear solution is evaporated. The residue is washed with tetrahydrofurane, filtered off and dried under vacuum. M.p. 256-259° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07531540B2uspto-grants-2009_05