Hydrochloric Acid → N-(3-Pyridinylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide

HRID 1830093Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1830093
COC([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH2:9][N:8]2[C:16]([C:19]([NH:21][CH2:22][C:23]3[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=3)=[O:20])=[CH:17][CH:18]=[C:7]2[CH2:6]1)=O.C(=O)([O-])[O-].[K+].[K+].O.Cl>CO>[N:25]1[CH:26]=[CH:27][CH:28]=[C:23]([CH2:22][NH:21][C:19]([C:16]2[N:8]3[C:7]([CH2:6][NH:5][C:11]4[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=4[CH2:9]3)=[CH:18][CH:17]=2)=[O:20])[CH:24]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 11430Potassium CarbonateHCID 2205365210-(Methoxycarbonyl)-N-(pyridin-3-ylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide

Produkt 1

HCID 22053658N-(3-Pyridinylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of 10-(methoxycarbonyl)-N-(pyridin-3-ylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide (5 mmol) of Step B in methanol (50 mL) was treated with potassium carbonate and stirred at room temperature overnight. Water was then added to the solution and the pH adjusted to 6 with 6N hydrochloric acid. The solution was extracted with ethyl acetate, and the combined organic layers were dried over anhydrous magnesium sulfate, and evaporated to dryness. The residual oil was triturated with ethyl acetate and hexane to yield the title compound as a powder.

Aufarbeitung

  1. extractionThe solution was extracted with ethyl acetate
  2. dry with materialthe combined organic layers were dried over anhydrous magnesium sulfate
  3. customevaporated to dryness
  4. customThe residual oil was triturated with ethyl acetate and hexane

Quellen und Nachweise

ORD-Eintrag
ord-aa39361e44fa45ee9f340f083efb44c7
Quelldatensatz
uspto-grants-2006_06
Patentnummer
US07064120B2

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