Potassium Hydroxide → 2,3,4,5-Tetrahydro-1,4-benzoxazepin-5-one

HRID 718102

Reaktionsgleichung

Reaktionsgleichung von HRID 718102
[O:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[CH2:3][CH2:2]1.[N-:12]=[N+]=[N-].[Na+].[OH-].[K+]>S(=O)(=O)(O)O>[O:1]1[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[C:4](=[O:11])[NH:12][CH2:3][CH2:2]1

Komponenten

5

Edukt 3

HCID 14797Potassium HydroxideHCID 33557Sodium AzideHCID 68110Chromanone

Produkt 1

HCID 3406292,3,4,5-Tetrahydro-1,4-benzoxazepin-5-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

The chroman-4-one (5.0 g, 33.8 mmol) was dissolved in sulfuric acid (10 mL) and the mixture was cooled at 0° C. Sodium azide (2.88 g, 44.3 mmol) was added portionwise followed by some sulfuric acid (5 mL). The reaction mixture was stirred at room temperature over night. The mixture was then pour into ice-water and basified to pH=7 with potassium hydroxide pellets. This aqueous layer was extracted with ether (twice).

Aufarbeitung

  1. extractionThis aqueous layer was extracted with ether (twice)

Quellen und Nachweise

ORD-Eintrag
ord-c15779cfa74d436daa5d0b80ddb66e44
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09193749B2

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