반응 #681560

ord-f26f03f4284c4415afb69594f0497f7c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed, under nitrogen, for 17 h
  2. 2
    여과the reaction mixture was filtered
  3. 3
    농축the filtrate was concentrated to dryness under reduced pressure
  4. 4
    기타Purification by FC (heptane/AcOEt=9/1)

실험 절차

A mixture of commercially available 2,5-dimethylbenzo[d]oxazole (1.000 g; 6.79 mmol), N-bromosuccinimide (1.209 g; 6.79 mmol), and commercially available dibenzoyl peroxide (11 mg; 0.046 mmol) in anh. CCl4 (10 ml) was refluxed, under nitrogen, for 17 h. After cooling to rt, the reaction mixture was filtered, and the filtrate was concentrated to dryness under reduced pressure. Purification by FC (heptane/AcOEt=9/1) afforded 5-(bromomethyl)-2-methylbenzo[d]oxazole as a yellow solid. LC-MS (conditions E): tR=0.61 min.; [M+H]+: 226.12 g/mol.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09242970B2uspto-grants-2016_01