Reaktion #2358259

Reaktionsgleichung

5-ethylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine

sodium hydride

methyl iodide

→

5-(N-ethylsulfonyl-N-methylamino)-2,3,4,5-tetrahydro-1-benzoxepine

Ausbeute 95.2%

Lösungsmittel

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITthe mixture was additionally stirred overnight at RT
2. 2
   workup.DISTILLATIONAfter distilling off the solvent
3. 3
   workup.ADDITIONthe residue was treated with water
4. 4
   Extraktionextracted with EA
5. 5
   EinengenThe organic phase was concentrated in vacuo
6. 6
   Trocknenafter drying over sodium sulfate

Vorschrift

A solution of 1.0 g (3.9 mmol) of 5-ethylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine in 15 ml of THF were added dropwise under nitrogen to a suspension of 0.16 g (5.4 mmol) of 80 percent sodium hydride in 10 ml of THF. After stirring at RT for 3 h, 1.6 g (11 mmol) of methyl iodide were added dropwise and the mixture was additionally stirred overnight at RT. After distilling off the solvent, the residue was treated with water and extracted with EA. The organic phase was concentrated in vacuo after drying over sodium sulfate. 1.0 g of 5-(N-ethylsulfonyl-N-methylamino)-2,3,4,5-tetrahydro-1-benzoxepine was obtained, m.p. 122-124° C.

Quelle