反応 #2457858

反応方程式

Lapatinib ditosylate

MeCN

MeCN

→

lapatinib ditosylate

N-(3-chloro-4-(3-fluorobenzyloxy)phenyl)-6-(5-((2-(methylsulfonyl) ethylamino)methyl)furan-2-yl)quinazolin-4-amine ditosylate

溶媒

DMSO

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred for 1 h
2. 2
   ろ過filtered
3. 3
   洗浄washed with MeCN (10 mL)
4. 4
   その他The filter cake was dried under vacuum at 60° C. for 16 h

実験手順

Lapatinib ditosylate (5.0 g, 5.4 mmol, 96.5% HPLC purity with the maximum individual impurity at 0.8%) was dissolved in DMSO (10 mL) at 70° C. (internal temperature). MeCN (10 mL) was added dropwise into the mixture at 70-80° C. (internal temperature) and was stirred at this temperature for 1 h. Over a 4 h period the mixture was cooled to room temperature. MeCN (30 mL) was added dropwise, and the mixture was stirred for 1 h, then filtered and washed with MeCN (10 mL). The filter cake was dried under vacuum at 60° C. for 16 h to give 4.0 g lapatinib ditosylate as crystalline Form 1 (as disclosed in U.S. Pat. No. 7,157,466 B2) with 99.6% HPLC purity in 78% HPLC yield.

出典