反応 #331996

ord-f7395c6d0b464896a2eb1c53acdd9e27

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Purification
  2. 2
    洗浄eluting with a linear gradient of 2-25% CMA in chloroform),
  3. 3
    その他followed by recrystallization from acetonitrile

実験手順

The general method described in Part A of Example 3 was followed using 7-bromo-2-ethoxymethyl-1-(2-hydroxy-2-methylpropyl)-1H-imidazo[4,5-c]quinolin-4-amine (U.S. Patent Application Publication No. US 2004/0147543, Examples 125-135) in lieu of 7-bromo-2-ethoxymethyl-1-(3-isopropoxypropyl)-1H-imidazo[4,5-c]quinoline and ethanesulfonamide in lieu of isobutyramide. Purification using a HORIZON HPFC system (silica cartridge, eluting with a linear gradient of 2-25% CMA in chloroform), followed by recrystallization from acetonitrile afforded 0.108 g of N-[4-amino-2-ethoxymethyl-1-(2-hydroxy-2-methylpropyl)-1H-imidazo[4,5-c]quinolin-7-yl]ethanesulfonamide as white crystals, mp 124.0-127.0° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08658666B2uspto-grants-2014_02