反応 #1106685

反応方程式

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

溶媒

DMF

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   その他The reaction mixture was partitioned between ethyl acetate and water
3. 3
   洗浄the ethyl acetate solution was washed with brine
4. 4
   乾燥dried (MgSO4)
5. 5
   その他evaporated in vacuo
6. 6
   その他to yield an oil
7. 7
   その他The oil was purified
8. 8
   その他to yield a white solid, which
9. 9
   その他was recrystallized (ethyl acetate/Hexane)

実験手順

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.

出典