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Sodium triacetoxyborohydride → 1-ethyl-3,3,5-trimethyl-7-(4-{N-[2-(2-methyl-4-oxo-4H-furo[3,2-c]pyridin-5-yl)ethyl]-N-(pyridin-4-ylmethyl)amino}butyl)-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione dihydrochloride

HRID 68957
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 68957
[CH3:1][C:2]1[O:10][C:9]2[CH:8]=[CH:7][N:6]([CH2:11][CH:12]=O)[C:5](=[O:14])[C:4]=2[CH:3]=1.[CH2:15]([N:17]1[C:23](=[O:24])[C:22]([CH3:26])([CH3:25])[C:21](=[O:27])[N:20]([CH3:28])[C:19]2[CH:29]=[C:30]([CH2:33][CH2:34][CH2:35][CH2:36][NH:37][CH2:38][C:39]3[CH:44]=[CH:43][N:42]=[CH:41][CH:40]=3)[CH:31]=[CH:32][C:18]1=2)[CH3:16].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(OC(=O)C)C.[ClH:65]>C(OCC)(=O)C.ClCCCl.C(O)(=O)C>[ClH:65].[ClH:65].[CH2:15]([N:17]1[C:23](=[O:24])[C:22]([CH3:26])([CH3:25])[C:21](=[O:27])[N:20]([CH3:28])[C:19]2[CH:29]=[C:30]([CH2:33][CH2:34][CH2:35][CH2:36][N:37]([CH2:12][CH2:11][N:6]3[CH:7]=[CH:8][C:9]4[O:10][C:2]([CH3:1])=[CH:3][C:4]=4[C:5]3=[O:14])[CH2:38][C:39]3[CH:40]=[CH:41][N:42]=[CH:43][CH:44]=3)[CH:31]=[CH:32][C:18]1=2)[CH3:16]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 5049666Sodium triacetoxyborohydrideHCID 21866389Hydrogen chloride-ethyl acetateHCID 706567041-Ethyl-3,3,5-trimethyl-7-{4-[(pyridin-4-ylmethyl)amino]butyl}-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dioneHCID 86670479(2-Methyl-4-oxo-4H-furo[3,2-c]pyridin 5-yl)acetaldehyde

Produkt 1

HCID 70656645
1-ethyl-3,3,5-trimethyl-7-(4-{N-[2-(2-methyl-4-oxo-4H-furo[3,2-c]pyridin-5-yl)ethyl]-N-(pyridin-4-ylmethyl)amino}butyl)-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 111,2-DichloroethaneLösungsmittelHCID 176Acetic AcidLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

(2-Methyl-4-oxo-4H-furo[3,2-c]pyridin 5-yl)acetaldehyde (0.18 g) and acetic acid (0.1 ml) were added to a 1,2-dichloroethane solution (5 ml) of 1-ethyl-3,3,5-trimethyl-7-{4-[(pyridin-4-ylmethyl)amino]butyl}-1,5-dihydrobenzo[b][1,4]diazepine 2,4-dione (0.38 g). The mixture was stirred for 30 minutes at room temperature. sodium triacetoxyborohydride (0.32 g) was added to the mixture, and the mixture was stirred at room temperature overnight. The reaction mixture was condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:methanol=1:0→9:1). The purified product was condensed under reduced pressure. A 6N-hydrogen chloride ethyl acetate solution (1.0 ml) was added to an ethyl acetate solution (20 ml) of the residue, and the liquid was stirred at room temperature. The precipitated insoluble matter was separated, washed with ethyl acetate, and dried to give the title compound (0.43 g) as a white solid.

Aufarbeitung

  1. stirringthe mixture was stirred at room temperature overnight
  2. customcondensed under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (ethyl acetate:methanol=1:0→9:1)
  4. customcondensed under reduced pressure
  5. stirringthe liquid was stirred at room temperature
  6. customThe precipitated insoluble matter was separated
  7. washwashed with ethyl acetate
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b42212217339456baee78b5a6ff9fa67
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08822453B2

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