反应 #531786

ord-b02e27fc945948d4979a75e5b131dc9b

反应方程式

O
water
N#CCc1ccc(N)cc1
4-aminobenzyl cyanide
c1ccncc1
pyridine
[Cl-]
chloride
CC1CCC(C(C)C)C(C(=O)Nc2ccc(CC#N)cc2)C1
desired product
CC1CCC(C(C)C)C(C(=O)Nc2ccc(CC#N)cc2)C1
N-(4-cyanomethylphenyl) p-menthanecarboxamide

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The mixture was separated
  2. 2
    洗涤The organic layer was washed with 50 mL of water and 50 mL of brine
  3. 3
    干燥The organic layer was dried over MgSO4
  4. 4
    其他The solvent was evaporated in vacuo
  5. 5
    其他to afford the crude product, which
  6. 6
    其他was recrystallized from hexanes

实验过程

To a flask, were added 6.6 g (50 mmol) of 4-aminobenzyl cyanide, 4.04 mL of pyridine and 100 mL MtBE. To this mixture, 10 g of p-menthane-3-carbon*yl chloride were added dropwise over 5 minutes. The reaction mixture was stirred for 24 h. To the reaction mixture, 50 mL of water were added. The mixture was separated. The organic layer was washed with 50 mL of water and 50 mL of brine. The organic layer was dried over MgSO4. The solvent was evaporated in vacuo to afford the crude product, which was recrystallized from hexanes to afford 10.1 g of the desired product with the following spectroscopic properties:

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE044339E1uspto-grants-2013_07