반응 #47788

반응 방정식

disulfanediyldibutane-4,1-diyl dimethane sulfonate

5,6,7,8-tetrahydroisoquinoline

potassium carbonate

→

2,2′-(disulfanediyldibutane-4,1-diyl)bis(5,6,7,8-tetrahydroisoquinolinium) dimethane sulfonate

용매

acetonitrile

acetonitrile

반응 조건

후처리

1. 1
   기타brought to 100° C
2. 2
   기타was brought back to ambient temperature
3. 3
   농축concentrated under vacuum
4. 4
   workup.ADDITION10 ml of dichloromethane were added
5. 5
   여과the solution was filtered
6. 6
   workup.ADDITIONpoured dropwise into 100 ml of ethyl ether
7. 7
   기타The oil that had separated
8. 8
   workup.ADDITIONby diluting in 10 ml of dichloromethane
9. 9
   workup.ADDITIONadding to 500 ml of ethyl ether
10. 10
    건조After drying under vacuum, 3.3 g of a brown oil
11. 11
    기타were recovered

실험 절차

2.1 g of 5,6,7,8-tetrahydroisoquinoline and 0.5 g of potassium carbonate were mixed in 2 ml of acetonitrile and brought to 100° C. A solution of 2.7 g of disulfanediyldibutane-4,1-diyl dimethane sulfonate in 2 ml of acetonitrile was added in 5 min. Stirring was maintained for 3 h at 100° C. and then the reaction medium was brought back to ambient temperature and concentrated under vacuum. 10 ml of dichloromethane were added and the solution was filtered and then poured dropwise into 100 ml of ethyl ether. The oil that had separated by settling out was reprocessed by diluting in 10 ml of dichloromethane and adding to 500 ml of ethyl ether. After drying under vacuum, 3.3 g of a brown oil were recovered. The analyses were in compliance with the expected structure.

출처