Cesium carbonate → HCID 59312356, Verbindung

HRID 2077058Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2077058
[CH2:1]([C:8]1[N:9]=[C:10](Cl)[C:11]2[CH2:17][CH2:16][N:15]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:14][CH2:13][C:12]=2[N:25]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:27](=O)([O-])[O-].[Cs+].[Cs+].CB1OB(C)OB(C)O1>O1CCOCC1>[CH2:1]([C:8]1[N:9]=[C:10]([CH3:27])[C:11]2[CH2:17][CH2:16][N:15]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:14][CH2:13][C:12]=2[N:25]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 10796Cesium carbonateHCID 574072TrimethylboroxineHCID 59312273HCID 59312273, Verbindung

Produkt 1

HCID 59312356HCID 59312356, VerbindungAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

2,7-dibenzyl-4-chloro-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine (70 mg, 0.193 mmol) of Preparation 38, Step B, was dissolved in dioxane (5 ml) and Caesium carbonate (251 mg, 0.77 mmol), trimethylboroxine (0.054 ml, 0.385 mmol) and Catalyst 1 (10 mg) were added. The reaction was refluxed under nitrogen for 3 h. The reaction was filtered over arbocel and diluted with ethyl acetate, washed with water, dried over MgSO4 filtered and concentrated in vacuo to afford the title compound as a colourless oil in 99% yield, 66 mg.

Aufarbeitung

  1. temperatureThe reaction was refluxed under nitrogen for 3 h
  2. filtrationThe reaction was filtered over arbocel
  3. additiondiluted with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7b92495c0826445ca0d47629a592ede7
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07928099B2

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