반응 #794984

반응 방정식

8-bromo-3,4-dihydrobenzo[b]oxepin-5(2H)-one

DMF

Phosphorus oxychloride

POCl3

DMF

→

(Z)-8-bromo-5-chloro-2,3-dihydrobenzo[b]oxepine-4-carbaldehyde

반응 조건

후처리

1. 1
   기타to reach room temperature
2. 2
   추출The aqueous phase was extracted with ethylacetate
3. 3
   세척the combined organics were washed with brine
4. 4
   건조dried over sodium sulfate
5. 5
   농축concentrated

실험 절차

Phosphorus oxychloride, POCl3 (1.88 mL, 20.8 mmol) was added dropwise to DMF (5 mL) at 0° C. After 30 min a solution of 8-bromo-3,4-dihydrobenzo[b]oxepin-5(2H)-one (2.0 g, 8.3 mmol) in 8 mL DMF was added dropwise. The reaction mixture was allowed to reach room temperature to stir 2 hr, then poured slowly over rapidly stirred ice water. The aqueous phase was extracted with ethylacetate and the combined organics were washed with brine, dried over sodium sulfate and concentrated to give (Z)-8-bromo-5-chloro-2,3-dihydrobenzo[b]oxepine-4-carbaldehyde.

출처