反应 #40375

ord-d40536500a4f4ac6b14cb0966f32001e

反应方程式

CCc1ccc(CC(C)(C)NC(C)=O)cc1
N-[2-(4-ethylphenyl)-1,1-dimethylethyl]acetamide
[K+].[OH-]
potassium hydroxide
Cl
hydrochloric acid
CCOCC
diethyl ether
CCc1ccc(CC(C)(C)N)cc1
2-(4-ethylphenyl)-1,1-dimethylethylamine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted three times with diethyl ether
  2. 2
    洗涤The combined organic phases are washed with water
  3. 3
    干燥dried with sodium sulfate
  4. 4
    其他To prepare the hydrochloride
  5. 5
    其他The solid precipitated
  6. 6
    过滤filtered
  7. 7
    其他dried

实验过程

16.3 g (74 mmol) of N-[2-(4-ethylphenyl)-1,1-dimethylethyl]acetamide and 8.0 g of potassium hydroxide are refluxed for 15 hours in 60 mL ethylene glycol. The reaction mixture is combined with ice water and extracted three times with diethyl ether. The combined organic phases are washed with water, dried with sodium sulfate, and freed from solvent. To prepare the hydrochloride, the crude product is dissolved in acetonitrile and ethereal hydrochloric acid and diethyl ether are added successively. The solid precipitated is suction filtered and dried. Yield: 11.0 g (69%, hydrochloride); melting point 165° C.-167° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07727984B2uspto-grants-2010_06