Sodium Hydroxide → 4-Cyclopropyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one

HRID 1525853Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1525853
Cl.[CH:2]1([N:5]2[CH2:10][C:9]3([CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)[O:8][CH2:7][C:6]2=[O:16])[CH2:4][CH2:3]1.[OH-].[Na+]>ClCCl.O>[CH:2]1([N:5]2[CH2:10][C:9]3([CH2:11][CH2:12][NH:13][CH2:14][CH2:15]3)[O:8][CH2:7][C:6]2=[O:16])[CH2:4][CH2:3]1

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 69083351HCID 69083351, Verbindung

Produkt 1

HCID 667837534-Cyclopropyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-oneAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A suspension of 4-cyclopropyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one hydrochloride (8.11 mmol) in dichloromethane (10 mL) was treated with 1N aq NaOH (10.00 mmol). The biphasic mixture was stirred for 1 hour, at which point the cloudy organic layer had turned clear. The contents of the flask were further diluted with water (50 mL) and dichloromethane (50 mL) and the layers were separated. The aqueous layer was extracted with dichloromethane. The organic layers were combined, dried over sodium sulfate, filtered and concentrated in vacuo to afford the title compound as a yellow oil (80%). MS(ES)+ m/e 211.2 [M+H]+.

Aufarbeitung

  1. customthe layers were separated
  2. extractionThe aqueous layer was extracted with dichloromethane
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-17f6540727ff438496b2f0e83f98c8a1
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09084794B2

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