Reaktion #2358258

ord-65e51f8995e14c3191e70cd612fa0e0d

Reaktionsgleichung

CCS(=O)(=O)Cl
ethanesulfonyl chloride
NC1CCCOc2ccccc21
5-amino-2,3,4,5-tetrahydro-1-benzoxepine
CCN(CC)CC
triethylamine
CCS(=O)(=O)NC1CCCOc2ccccc21
5-ethylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine
Ausbeute 70.6%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto come to room temperature
  2. 2
    workup.DISTILLATIONthe solvent was distilled off in vacuo
  3. 3
    workup.STIRRINGAfter stirring the residue with water
  4. 4
    Filtrationthe deposited product was filtered off with suction

Vorschrift

0.86 g (6.7 mmol) of ethanesulfonyl chloride was added dropwise with ice cooling to a solution of 1.0 g (6.1 mmol) of 5-amino-2,3,4,5-tetrahydro-1-benzoxepine and 2.5 g (24 mmol) of triethylamine in 20 ml of THF. The mixture was allowed to come to room temperature and was stirred overnight, and the solvent was distilled off in vacuo. After stirring the residue with water, the deposited product was filtered off with suction. 1.1 g of 5-ethylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine were obtained, m.p. 109-111° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06333349B1uspto-grants-2001_12