تفاعل #730779

معادلة التفاعل

3,5-bis-(trifluoromethyl)-bromobenzene

methyl 2-acetylamino-acrylate

tri-o-tolyl-phosphane

→

methyl 2-acetylamino-3-(3,5-bis-trifluoromethyl-phenyl)acrylate

المذيبات

triethylamine

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   أخرىwas evaporated down i
2. 2
   ترشيحfiltered
3. 3
   أخرىthe phases were separated
4. 4
   تجفيفThe organic phase was dried over Na2SO4
5. 5
   ترشيحfiltered
6. 6
   أخرىevaporated to dryness
7. 7
   workup.STIRRINGThe residue was stirred with DIPE, suction
8. 8
   ترشيحfiltered
9. 9
   أخرىdried i

الإجراء التجريبي

Under a nitrogen atmosphere 50.0 g (171 mmol) 3,5-bis-(trifluoromethyl)-bromobenzene, 25.0 g (171 mmol) methyl 2-acetylamino-acrylate in 475 mL triethylamine and 250 mL acetonitrile were combined with 3.9 g (12.4 mmol) tri-o-tolyl-phosphane and 2.8 g (12.5 mmol) Pd(OAc)2 and stirred for 18 h at 80° C. After the reaction had ended the reaction mixture was evaporated down i. vac. to approx. 200 mL, combined with 400 mL EtOAc and 400 mL water, the precipitate was suction filtered and the phases were separated. The organic phase was dried over Na2SO4, combined with activated charcoal, filtered and evaporated to dryness. The residue was stirred with DIPE, suction filtered and dried i. vac.

المصدر