Reaktion #2075756

Reaktionsgleichung

2-(7-Hydroxymethyl-9H-thioxanthen-4-yl)-6-morpholin-4-yl-pyran-4-one

hydrogen bromide

→

crude title compound

Ausbeute 100.0%

2-(7-Bromomethyl-9H-thioxanthen-4-yl)-6-morpholin-4-yl-pyran-4-one

Ausbeute 100.0%

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeby bubbling hydrogen bromide gas through the reaction mixture until the solution
2. 2
   Sonstigehydrogen bromide gas was again bubbled through the reaction mixture
3. 3
   WaschenThe reaction mixture was washed with saturated NaHCO3 and water
4. 4
   TrocknenThe organic layer was dried over MgSO4
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated in vacuo
7. 7
   SonstigeThe brown coloured solid was dried under vacuum at 50° C.

Vorschrift

A solution of 2-(7-Hydroxymethyl-9H-thioxanthen-4-yl)-6-morpholin-4-yl-pyran-4-one (3)(240 mg, 0.59 mmol) in chloroform (10 mL) was saturated with hydrogen bromide by bubbling hydrogen bromide gas through the reaction mixture until the solution became cloudy. After 18 hours, hydrogen bromide gas was again bubbled through the reaction mixture. The reaction mixture was washed with saturated NaHCO3 and water. The organic layer was dried over MgSO4, filtered and concentrated in vacuo. The brown coloured solid was dried under vacuum at 50° C. to give the crude title compound (assumed 100%) which was used without any further purification. m/z (LC-MS, ESP): 470.2 [M+H]+ (1:1, bromine isotope ratio present), R/T=3.86 mins

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