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

HRID 1946632

Reaktionsgleichung

Reaktionsgleichung von HRID 1946632
[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×

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 oC. 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. temperaturethe mixture was cooled at 0 oC
  2. extractionThis aqueous layer was extracted with ether (twice)

Quellen und Nachweise

ORD-Eintrag
ord-88a9b647d76b4d0aa3e7a773eadd29f4
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08399452B2

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