반응 #7586

ord-1ef1353ef9b0448aa2e55a73c9130f30

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타(prepared
  2. 2
    온도at reflux for 3 hours
  3. 3
    여과the resulting solid filtered off
  4. 4
    세척washed with ether

실험 절차

A suspension of 4-chloro-6-methoxy-7-[( 1-methylimidazol-2-yl)methoxy]cinnoline (109 mg, 0.35 mmol) and 2-fluoro-5-hydroxy-4-methylaniline (70 mg, 0.5 mmol), (prepared as described for the starting material in Example 11), in 2-pentanol (3 ml), DMF (0.5 ml) and a 5M solution of hydrogen chloride in isopropanol (74 μl, 0.35 mmol) was heated at reflux for 3 hours. The solution was then cooled to 0° C. and the resulting solid filtered off and washed with ether to give 4-(2-fluoro-5-hydroxy-4-methylanilino)-6-methoxy-7-[(1-methylimidazol-2-yl)methoxy]cinnoline hydrochloride as a yellow solid (124 mg, 73%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087602B2uspto-grants-2006_08