تفاعل #60928

معادلة التفاعل

3-chloro-4-iodobenzotrifluoride

N-Boc-piperazine

sodium-t-butoxide

tri-o-tolylphosphine

→

title compound

المردود 10.0%

1-(2-Chloro-4-trifluoromethyl-phenyl)piperazine

المردود 10.0%

المذيبات

ether

dioxane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto cool to room temperature
2. 2
   غسيلwashed with brine (25 ml)
3. 3
   تجفيفThe organic layer was dried over Na2SO4
4. 4
   ترشيحfiltered
5. 5
   أخرىthe solvent was removed in vacuo
6. 6
   أخرىThe crude oil was chromatographed over on silica gel

الإجراء التجريبي

A mixture of 0.5 g (1.6 mmol) of 3-chloro-4-iodobenzotrifluoride 0.7 g (3.8 mmol), N-Boc-piperazine, 41 mg (0.04 mmol) Tris(dibenzylideneacetone)dipalladium chloroform complex, 0.44 g (4.43 mmol) sodium-t-butoxide and 48 mg (0.16 mmol) tri-o-tolylphosphine in 6 ml dioxane was heated overnight at 100° C. The solution was allowed to cool to room temperature, taken up in ether (30 ml) and washed with brine (25 ml). The organic layer was dried over Na2SO4, filtered and the solvent was removed in vacuo. The crude oil was chromatographed over on silica gel: Eluent: Heptane-AcOEt 0-10% over 15 min to provide the title compound (0.06 g, 10%) as a brown oil, MS (m/e): 365.1 (MH+, 100%).

المصدر