反应 #684950

ord-a3f2ef2235d34a34a297f4e40f54e2a9

反应方程式

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
收率 55.3%
CCCCc1ccc(Cc2nccc3ccccc23)cc1
1-(4-Butylbenzyl)Isoquinoline
收率 55.3%

反应条件

温度
160°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.WAITat 200° C. for 1 hour
  2. 2
    温度The mixture was cooled to room temperature
  3. 3
    萃取this was extracted with ethyl acetate
  4. 4
    洗涤The extract was washed with water
  5. 5
    干燥dried over anhydrous magnesium sulfate
  6. 6
    浓缩concentrated under reduced pressure
  7. 7
    其他The residue was purified by silica gel column chromatography

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07897387B2uspto-grants-2011_03