تفاعل #446167

معادلة التفاعل

sodium ethoxide

2-chloromethyl-3,5-dicarboethoxy-4-(m-nitrophenyl) -6-methyl-1,4-dihydropyridine

H2SO4

hydrogen sulfide

→

2-mercaptomethyl-3,5-dicarboethoxy-4-(m-nitrophenyl) -6-methyl-1,4-dihydropyridine

المذيبات

water

DME

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe reaction mixture is warmed to 0° C.
2. 2
   ترشيحThe precipitate is filtered off
3. 3
   أخرىdried in vacuum
4. 4
   أخرىrecrystallized from Et2O

الإجراء التجريبي

A stirred ethanolic solution (200 ml) of an alkaline alkoxide, for example sodium ethoxide (20 g), is saturated, at +10° C., with dry hydrogen sulfide, cooled to -15° C., and added with a solution of 2-chloromethyl-3,5-dicarboethoxy-4-(m-nitrophenyl) -6-methyl-1,4-dihydropyridine (25 g) in DME (70 ml). After one hour, the reaction mixture is warmed to 0° C., acidified with H2SO4 (10% water solution; 100 ml) and diluted with water (1400 ml). The precipitate is filtered off, dried in vacuum, and recrystallized from Et2O to give 23 g of 2-mercaptomethyl-3,5-dicarboethoxy-4-(m-nitrophenyl) -6-methyl-1,4-dihydropyridine, m.p. 145°-147° C.

المصدر