反応 #1131898

反応方程式

lapatinib

Lapatinib

lapatinib ditosylate

lapatinib ditosylate

→

lapatinib ditosylate

p-toluenesulfonic acid

反応条件

後処理

1. 1
   その他can be isolated
2. 2
   その他reaction product mixture
3. 3
   その他The reaction product mixture from the step iii) is quenched with a basic aqueous solution such as aq. NaOH
4. 4
   その他separated
5. 5
   洗浄the organic phase is washed with an acidic aqueous solution such as aq. NH4Cl
6. 6
   ろ過The organic phase is then filtered

実験手順

Lapatinib prepared using the method of this embodiment can be isolated, or more preferably it can be directly converted into highly pure lapatinib ditosylate salt without isolation of the lapatinib from the step iii) reaction product mixture. The isolated lapatinib ditosylate has a HPLC purity of 97.0-99.9%, preferably >99.0%, most preferably >99.8%. The reaction product mixture from the step iii) is quenched with a basic aqueous solution such as aq. NaOH, separated and the organic phase is washed with an acidic aqueous solution such as aq. NH4Cl. The organic phase is then filtered and lapatinib ditosylate as crystalline Form I is obtained by crystallisation from the organic phase in the presence of p-toluenesulfonic acid. The lapatinib ditosylate is isolated by filtration or centrifugation, or other methods of solid isolation.

出典