تفاعل #1106685

معادلة التفاعل

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

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   أخرىThe reaction mixture was partitioned between ethyl acetate and water
3. 3
   غسيلthe ethyl acetate solution was washed with brine
4. 4
   تجفيفdried (MgSO4)
5. 5
   أخرىevaporated in vacuo
6. 6
   أخرىto yield an oil
7. 7
   أخرىThe oil was purified
8. 8
   أخرىto yield a white solid, which
9. 9
   أخرىwas recrystallized (ethyl acetate/Hexane)

الإجراء التجريبي

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.

المصدر