تفاعل #554699

معادلة التفاعل

1,1,1-trifluoro-2,3-epoxypropane

benzyl piperazine-1-carboxylate

1,1,1-trifluoro-2,3-epoxypropane

→

expected compound

Benzyl 4-(3,3,3-trifluoro-2-hydroxypropyl)piperazine-1-carboxylate

المذيبات

N-methylpyrrolidine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةit is heated at 80° C. for 48 hours
2. 2
   استخلاصThe reaction mixture is extracted with DCM
3. 3
   غسيلthe organic phase is washed with a 4% solution of LiCl in water, it
4. 4
   تجفيفis dried over MgSO4
5. 5
   أخرىthe solvent is evaporated under vacuum
6. 6
   أخرىThe residue is purified by preparative HPLC

الإجراء التجريبي

0.47 ml of 1,1,1-trifluoro-2,3-epoxypropane is added to a solution of 1 g of benzyl piperazine-1-carboxylate in 100 ml of N-methylpyrrolidine and it is heated at 80° C. for 12 hours. 0.05 ml of 1,1,1-trifluoro-2,3-epoxypropane is added and it is heated at 80° C. for 48 hours, The reaction mixture is extracted with DCM, the organic phase is washed with a 4% solution of LiCl in water, it is dried over MgSO4 and the solvent is evaporated under vacuum. The residue is purified by preparative HPLC and 1.7 g of the expected compound is obtained.

المصدر