Hydrochloric Acid → 4-(3-Piperidin-1-yl-propyl)-[1,4]diazepan-5-one dihydrochloride

HRID 1867359Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1867359
C(OC([N:8]1[CH2:14][CH2:13][C:12](=[O:15])[N:11]([CH2:16][CH2:17][CH2:18][N:19]2[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:25].CO>C(Cl)Cl.O1CCOCC1>[ClH:25].[ClH:25].[N:19]1([CH2:18][CH2:17][CH2:16][N:11]2[C:12](=[O:15])[CH2:13][CH2:14][NH:8][CH2:9][CH2:10]2)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24]1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 66783496HCID 66783496, Verbindung

Produkt 1

HCID 670807474-(3-Piperidin-1-yl-propyl)-[1,4]diazepan-5-one dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of 7.3 g (21.50 mmol) of 5-oxo-4-(3-piperidin-1-yl-propyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester was dissolved in 140 ml CH2Cl2, cooled to 0° C. and treated with 54 ml (215.03 mmol) of 4M HCl in dioxane, then warmed to RT. After 3 h, 40 ml of MeOH were added to dissolve the precipitation and stirring was continued over night. The solution was evaporated, dissolved in toluene and evaporated (2×) to yield 7.71 g (quantitative) of the title compound as a white solid. MS: 240.1 (MH+).

Aufarbeitung

  1. temperaturewarmed to RT
  2. dissolutionto dissolve
  3. customthe precipitation
  4. waitwas continued over night
  5. customThe solution was evaporated
  6. dissolutiondissolved in toluene
  7. customevaporated (2×)

Quellen und Nachweise

ORD-Eintrag
ord-6f5c80cb758041f7b03a362c62d0a878
Quelldatensatz
uspto-grants-2009_12
Patentnummer
US07632829B2

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