反应 #75876

ord-08d6d8aa25df402e84fb3648a2237202

反应方程式

CCOC(=O)C1=C(COCCN)NC(C)=C(C(=O)OC)C1c1ccccc1Cl
Amlodipine free base
O=C(O)c1cccnc1
Nicotinic acid
CCOC(=O)C1=C(COCCN)NC(C)=C(C(=O)OC)C1c1ccccc1Cl
amlodipine
CCOC(=O)C1=C(COCCN)NC(C)=C(C(=O)OC)C1c1ccccc1Cl.O=C([O-])c1cccnc1
amlodipine nicotinate
收率 85.0%

溶剂

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was heated
  2. 2
    温度at reflux
  3. 3
    workup.DISSOLUTIONwas completely dissolved
  4. 4
    其他The solids formed
  5. 5
    其他were isolated by filtration
  6. 6
    洗涤washed with ethyl acetate
  7. 7
    其他dried under reduced pressure

实验过程

Amlodipine free base (4.09 g) was added to 40 mL of ethanol. The mixture was heated at reflux and stirred until the solid was completely dissolved. Nicotinic acid (1.23 g) was added to the amlodipine solution and then the mixture was slowly cooled down to 0° C. within one hour. The solids formed were isolated by filtration, washed with ethyl acetate and dried under reduced pressure to yield 4.51 g of amlodipine nicotinate.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06699892B2uspto-grants-2004_03