반응 #1161235

반응 방정식

ethanol

Ethyl 2-mercaptoacetate

α-bromo-p-xylene

sodium ethylate

→

Ethyl (4-methylbenzylthio)acetate

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.WAITThe mixture is left
2. 2
   workup.ADDITIONis then added in the course of 20 minutes at a temperature in the region of 20° C
3. 3
   온도is maintained for 60 minutes at this temperature
4. 4
   기타the reaction mixture is then evaporated to dryness at 50° C. under reduced pressure (20 mm Hg; 2.7 kPa)
5. 5
   기타The residue obtained
6. 6
   건조the organic phase is dried over anhydrous magnesium sulphate
7. 7
   여과filtered
8. 8
   농축concentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa)

실험 절차

Ethyl 2-mercaptoacetate (8.5 cc) is added in the course of 15 minutes at a temperature in the region of 20° C. to a stirred solution, through which a stream of nitrogen is passed, of a 2M ethanolic solution of sodium ethylate (37.5 cc) and ethanol (50 cc). The mixture is left with stirring for 15 minutes at the same temperature, and α-bromo-p-xylene (13.9 g) is then added in the course of 20 minutes at a temperature in the region of 20° C. Stirring is maintained for 60 minutes at this temperature, and the reaction mixture is then evaporated to dryness at 50° C. under reduced pressure (20 mm Hg; 2.7 kPa). The residue obtained is dissolved in dichloromethane (100 cc), and the organic phase is dried over anhydrous magnesium sulphate, filtered and concentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa). Ethyl (4-methylbenzylthio)acetate (15.6 g) is thereby obtained, and is used in the crude state in the subsequent syntheses.

출처