반응 #1106685

반응 방정식

Racemic 2,3-dihydro-1,4-benzdioxin-2-ylmethylamine

triethylamine

dimethylsulfamoyl chloride

→

title compound

N-(2,3-Dihydro-benzo[1,4]dioxin-2-ylmethyl)-N′,N′dimethylsulfamide

용매

DMF

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타The reaction mixture was partitioned between ethyl acetate and water
3. 3
   세척the ethyl acetate solution was washed with brine
4. 4
   건조dried (MgSO4)
5. 5
   기타evaporated in vacuo
6. 6
   기타to yield an oil
7. 7
   기타The oil was purified
8. 8
   기타to yield a white solid, which
9. 9
   기타was recrystallized (ethyl acetate/Hexane)

실험 절차

Racemic 2,3-dihydro-1,4-benzdioxin-2-ylmethylamine (8.25 g, 5.0 mmol) and triethylamine (1.52 g, 15 mmol) were combined in DMF (10 mL) and cooled in an ice bath as dimethylsulfamoyl chloride (1.44 g, 10 mmol) was added. The reaction mixture was then stirred for 3 hr with continued cooling. The reaction mixture was partitioned between ethyl acetate and water, and the ethyl acetate solution was washed with brine, dried (MgSO4) and evaporated in vacuo to yield an oil. The oil was purified using flash column chromatography (ethyl acetate:Heptane—1:1) to yield a white solid, which was recrystallized (ethyl acetate/Hexane) to yield the title compound as a white floccular solid.

출처