Reaktion #795288

Reaktionsgleichung

1-(1-hydroxy-2-methylpropan-2-yl)thiourea

4,8-dibromo-3,4-dihydro-2Hbenzo[b]oxepin-5-one

→

2-(8-Bromo-4,5-dihydrothiazolo[4,5-d]benzo[b]oxepine-2-ylamino)-2-methylpropan-1-ol

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux for 3 hours
3. 3
   EinengenThe mixture was concentrated
4. 4
   Sonstigethe residue purified on silica gel column
5. 5
   Wascheneluting the product with 10% of methanol in dichloromethane

Vorschrift

A mixture of 0.67 g (5.0 mmol) of 1-(1-hydroxy-2-methylpropan-2-yl)thiourea and 1.60 g (5.00 mmol) of 4,8-dibromo-3,4-dihydro-2Hbenzo[b]oxepin-5-one in 30 ml of ethanol was heated under reflux for 3 hours. The mixture was concentrated, the residue purified on silica gel column eluting the product with 10% of methanol in dichloromethane. Yield 1.38 g (75%). MS(ESI+): 369.3

Quelle