반응 #1583832

ord-ce787ebc0d7647ec85ebece5eb44062b

반응 방정식

Cc1cc(I)ccc1Cl
2-chloro-5-iodotoluene
O=C1CCC(=O)N1Br
N-bromosuccinimide
Clc1ccc(I)cc1CBr
title compound
수율 97.3%
Clc1ccc(I)cc1CBr
2-(bromomethyl)-1-chloro-4-iodobenzene
수율 97.3%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction mixture was irradiated with a halogen sun lamp (150 watt) for 2 h
  2. 2
    기타The two-phase reaction mixture
  3. 3
    기타was separated
  4. 4
    추출the aqueous layer was extracted with dichloromethane (50 mL)
  5. 5
    세척The combined organic layers were washed with water (2×150 mL)
  6. 6
    건조dried over magnesium sulfate
  7. 7
    여과filtered
  8. 8
    농축concentrated under reduced pressure

실험 절차

To a mixture of 2-chloro-5-iodotoluene (4.07 g, 16.12 mmol), N-bromosuccinimide (3.16 g, 17.73 mmol) in dichloromethane (258 mL) and water (258 mL) was added 2,2′-azodiisobutyronitrile (0.132 g, 0.81 mmol). The reaction mixture was irradiated with a halogen sun lamp (150 watt) for 2 h and then cooled to room temperature. The two-phase reaction mixture was separated, and the aqueous layer was extracted with dichloromethane (50 mL). The combined organic layers were washed with water (2×150 mL), dried over magnesium sulfate, filtered and concentrated under reduced pressure to provide the title compound as an orange oil (5.20 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09198433B2uspto-grants-2015_12