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Sodium Bicarbonate → HCID 90166363, Verbindung

HRID 1486767
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1486767
[NH:1]([C:3]1[N:8]=[C:7]([CH3:9])[N:6]=[C:5]([C@@H:10]2[CH2:12][C@H:11]2[C:13]2[N:17]([CH3:18])[C:16]3[CH:19]=[CH:20][CH:21]=[CH:22][C:15]=3[N:14]=2)[CH:4]=1)[NH2:2].[Si:23]([O:30][C@@H:31]([CH3:40])[C:32]([N:34]=[C:35](N(C)C)[CH3:36])=O)([C:26]([CH3:29])([CH3:28])[CH3:27])([CH3:25])[CH3:24].C(=O)(O)[O-].[Na+]>C(O)(=O)C.COCCOC>[Si:23]([O:30][C@H:31]([C:32]1[N:1]([C:3]2[N:8]=[C:7]([CH3:9])[N:6]=[C:5]([C@@H:10]3[CH2:12][C@H:11]3[C:13]3[N:17]([CH3:18])[C:16]4[CH:19]=[CH:20][CH:21]=[CH:22][C:15]=4[N:14]=3)[CH:4]=2)[N:2]=[C:35]([CH3:36])[N:34]=1)[CH3:40])([C:26]([CH3:29])([CH3:28])[CH3:27])([CH3:25])[CH3:24]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 516892Sodium Bicarbonate2×HCID 86732071HCID 86732071, VerbindungHCID 90157317(S)-2-((tert-butyldimethylsilyl)oxy)-N-(1-(dimethylamino)ethylidene)propanamide

Produkt 1

HCID 90166363HCID 90166363, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittel
HCID 80711,2-DimethoxyethaneLösungsmittel

Versuchsvorschrift

To a solution of Intermediate 6 (1.8 g, 6.1 mmol) in acetic acid (40 ml) was added Intermediate 13 (4.0 g, 14.7 mmol) as a crude reaction mixture in 1,2-dimethoxyethane (40 mL). The reaction mixture was allowed to stir for 5 minutes at room temperature and then heated at 80° C. for 1 h. The reaction was cooled to room temperature, poured carefully over saturated aqueous sodium bicarbonate solution (200 mL), and the aqueous layer was made basic to pH˜8 by the addition of solid sodium bicarbonate. The solution was extracted with ethyl acetate (200 mL) and the organic layer was dried over sodium sulfate, filtered and concentrated. The crude product was purified by silica gel chromatography (0-60% EtOAc/hexanes) to afford 13-1 as an oil. MS: m/z=504.4 (M+H).

Aufarbeitung

  1. temperatureheated at 80° C. for 1 h
  2. temperatureThe reaction was cooled to room temperature
  3. extractionThe solution was extracted with ethyl acetate (200 mL)
  4. dry with materialthe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude product was purified by silica gel chromatography (0-60% EtOAc/hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-77927ba6493b441cb02f114eef5310be
Quelldatensatz
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09428492B2

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