Reaktion #2278175

Reaktionsgleichung

Tert-butyl [6-(tert-butoxycarbonylamino)methyl-3-ethylbicyclo[3.2.0]hept-3-en-6-yl]acetate

thioanisole

p-toluenesulfonic acid monohydrate

→

powder

Ausbeute 59.1%

[6-Aminomethyl-3-ethylbicyclo[3.2.0]hept-3-en-6-yl]acetic acid p-toluenesulfonate

Ausbeute 59.1%

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux
2. 2
   workup.WAITThe mixture was left
3. 3
   workup.WAITstanding overnight at room temperature
4. 4
   Filtrationthe resulting powder was collected by filtration
5. 5
   WaschenThe obtained powder was washed with ethyl acetate
6. 6
   Sonstigedried

Vorschrift

Tert-butyl [6-(tert-butoxycarbonylamino)methyl-3-ethylbicyclo[3.2.0]hept-3-en-6-yl]acetate (1152.23 g, 391.6 mmol) was dissolved in benzene (1.2 L). To the solution, thioanisole (145.57 g, 1173 mmol) and p-toluenesulfonic acid monohydrate (89.39 g) were then added, and the mixture was stirred for 2 hours under reflux. The mixture was left standing overnight at room temperature, and the resulting powder was collected by filtration. The obtained powder was washed with ethyl acetate and then dried to obtain the compound of interest as a white powder (88.29 g, 59%).

Quelle