반응 #1672672

반응 방정식

(3RS)-1-benzyl-3-hydroxymethyl pyrrolidine

thionyl chloride

→

(3RS)-1-benzyl-3-chloromethyl pyrrolidine

용매

CHCl3

CHCl3

반응 조건

후처리

1. 1
   기타The mixture was evaporated
2. 2
   workup.DISSOLUTIONthe residue was dissolved in water
3. 3
   세척The water layer was washed with ethyl acetate
4. 4
   추출The water layer was extracted three times with ethyl acetate
5. 5
   건조the combined organic layer was dried (Na2SO4)
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   기타to give the product in a quantitative yield (16.8 g)

실험 절차

To a refluxing solution of 15.3 g (0.08 mole) (3RS)-1-benzyl-3-hydroxymethyl pyrrolidine in 220 ml CHCl3 was slowly added a solution of 330 ml thionyl chloride in 60 ml CHCl3, and the reflux was continued for one hour. The mixture was evaporated and the residue was dissolved in water. The water layer was washed with ethyl acetate and then made alkaline with 0.2 M NaOH-solution. The water layer was extracted three times with ethyl acetate and the combined organic layer was dried (Na2SO4), filtered and evaporated to give the product in a quantitative yield (16.8 g).

출처