반응 #323754

반응 방정식

1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-carboxylic acid imidazolide

mercaptoethanol

tetrahydrofuran

→

yellow foam

β-Hydroxy-ethyl 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-thiocarboxylate

반응 조건

후처리

1. 1
   농축The mixture is concentrated
2. 2
   농축the concentrate is concentrated at 70° C.
3. 3
   workup.DISSOLUTIONthe residue is dissolved in chloroform
4. 4
   세척the solution is washed twice with water
5. 5
   기타dried
6. 6
   농축concentrated
7. 7
   기타The resulting evaporation residue
8. 8
   기타is purified over a silica gel column with a volume of 160 ml

실험 절차

3 g of 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-carboxylic acid imidazolide are boiled in 12.5 ml of absolute tetrahydrofuran with 5 ml of mercaptoethanol for 7 hours. The mixture is concentrated, the concentrate is concentrated at 70° C. using an oil pump, the residue is dissolved in chloroform and the solution is washed twice with water, dried and concentrated. The resulting evaporation residue is purified over a silica gel column with a volume of 160 ml, using toluene and later toluene/ethyl acetate 6:1 as the mobile phase. 1.94 g of a yellow foam with an Rf value of 0.25 are obtained as the main fraction.

출처