반응 #684950

ord-a3f2ef2235d34a34a297f4e40f54e2a9

반응 방정식

CCCCc1ccc(C(=O)c2nccc3ccccc23)cc1
compound
CCCCc1ccc(C(=O)c2nccc3ccccc23)cc1
(4-Butylphenyl)(1-isoquinolyl)ketone
NN.O
hydrazine monohydrate
[K+].[OH-]
potassium hydroxide
CCCCc1ccc(Cc2nccc3ccccc23)cc1
title compound
수율 55.3%
CCCCc1ccc(Cc2nccc3ccccc23)cc1
1-(4-Butylbenzyl)Isoquinoline
수율 55.3%

반응 조건

온도
160°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITat 200° C. for 1 hour
  2. 2
    온도The mixture was cooled to room temperature
  3. 3
    추출this was extracted with ethyl acetate
  4. 4
    세척The extract was washed with water
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    농축concentrated under reduced pressure
  7. 7
    기타The residue was purified by silica gel column chromatography

실험 절차

The compound of Example B3 (1.7 g, 6.0 mmol), hydrazine monohydrate (836 mg, 17 mmol), and potassium hydroxide (769 mg, 14 mmol) were added to diethylene glycol (8.5 ml), and this mixture was stirred at 80° C. for 1 hour, at 160° C. for 3.5 hours, then at 200° C. for 1 hour. The mixture was cooled to room temperature, ice water was added, and this was extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (914 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07897387B2uspto-grants-2011_03