Reaktion #715080

Reaktionsgleichung

4,5-dihydrobenzo[b]thieno[2,3-d]oxepine

acetic acid

N-bromosuccinimide

→

2-bromo-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeReaction mixture
2. 2
   Einengenbefore being concentrated in-vacuo
3. 3
   workup.DISSOLUTIONResidue was dissolved in ethyl acetate
4. 4
   WaschenOrganic phase was washed with water and brine
5. 5
   Trocknendried (Na2SO4)
6. 6
   Einengenconcentrated in-vacuo

Vorschrift

To a stirred solution of 4,5-dihydrobenzo[b]thieno[2,3-d]oxepine (440 mg, 2.2 mmol) and acetic acid (10 ml) in dichloromethane (10 ml) at 0° C., was added N-bromosuccinimide in portions. Reaction mixture was stirred for 18 hours, allowing solution to raise to room temperature before being concentrated in-vacuo. Residue was dissolved in ethyl acetate and sat. sodium carbonate solution. Organic phase was washed with water and brine, dried (Na2SO4) and concentrated in-vacuo to give 2-bromo-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine.

Quelle