반응 #430459

ord-63b1db53595e48458e37f1fae887e54d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed
  2. 2
    기타illuminated with sunlamp for 2 hours
  3. 3
    온도The resulting suspension was cooled
  4. 4
    여과filtered
  5. 5
    기타the filter cake was triturated with methanol
  6. 6
    기타to give 9.9 g, (85%) of the methanol-insoluble ethyl 3-bromomethyl-5-chlorobenzo(b)thiophene-2-carboxylate

실험 절차

A mixture of ethyl 5-chloro-3-methylbenzo(b)thiophene-2-carboxylate (9.0 g, 0.035 mol), N-bromosuccinimide (6.53 g, 0.037 mol) and benzoyl peroxide (130 mg) in carbon tetrachloride (150 ml) was refluxed and illuminated with sunlamp for 2 hours. The resulting suspension was cooled, filtered and the filter cake was triturated with methanol to give 9.9 g, (85%) of the methanol-insoluble ethyl 3-bromomethyl-5-chlorobenzo(b)thiophene-2-carboxylate: mp 148°-150° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05861309uspto-grants-1999_01