Isopropanol → 4-(4-Chloro-2-fluoro-5-hydroxyanilino)-6-methoxy-7-(4-pyridylmethoxy)cinnoline

HRID 7475

反応式

HRID 7475 の反応式
Cl.Cl[C:3]1[C:12]2[C:7](=[CH:8][C:9]([O:15][CH2:16][C:17]3[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=3)=[C:10]([O:13][CH3:14])[CH:11]=2)[N:6]=[N:5][CH:4]=1.[Cl:23][C:24]1[C:30]([OH:31])=[CH:29][C:27]([NH2:28])=[C:26]([F:32])[CH:25]=1.C(O)(C)C>CC(O)CCC>[Cl:23][C:24]1[C:30]([OH:31])=[CH:29][C:27]([NH:28][C:3]2[C:12]3[C:7](=[CH:8][C:9]([O:15][CH2:16][C:17]4[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=4)=[C:10]([O:13][CH3:14])[CH:11]=3)[N:6]=[N:5][CH:4]=2)=[C:26]([F:32])[CH:25]=1

参加物

5

反応物 3

HCID 3776IsopropanolHCID 1586545-Amino-2-chloro-4-fluorophenolHCID 219910114-Chloro-6-methoxy-7-(4-pyridylmethoxy)cinnoline hydrochloride

生成物 1

HCID 219910264-(4-Chloro-2-fluoro-5-hydroxyanilino)-6-methoxy-7-(4-pyridylmethoxy)cinnoline

試薬・触媒・溶媒 1

HCID 223862-Pentanol溶媒

実験手順

A suspension of 4-chloro-6-methoxy-7-(4-pyridylmethoxy)cinnoline hydrochloride (0.17 g, 0.45 mmol) and 4-chloro-2-fluoro-5-hydroxyaniline (102 mg, 0.63 mmol), (prepared as described in EP 061741 A2), in 2-pentanol (3.5 ml) was heated at reflux overnight. After cooling, isopropanol was added. The solid formed was filtered off, washed with isopropanol, ether and dried under vacuum to give 4-(4-chloro-2-fluoro-5-hydroxyanilino)-6-methoxy-7-(4-pyridylmethoxy)cinnoline as the hydrochloride salt (yellow solid, 194 mg, 86%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. temperatureAfter cooling
  4. customThe solid formed
  5. filtrationwas filtered off
  6. washwashed with isopropanol, ether
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-0d9c8fe8bd4f4677b9f2be711a09a26f
出典データセット
uspto-grants-2006_08
特許番号
US07087602B2

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