Ethylenediamine → 7-(2-Aminoethyl)amino-1-(5-amino-2,4-difluorophenyl)-8-chloro-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid

HRID 369226ノート

反応式

HRID 369226 の反応式
[NH2:1][C:2]1[C:3]([F:26])=[CH:4][C:5]([F:25])=[C:6]([N:8]2[C:17]3[C:12](=[CH:13][C:14]([F:20])=[C:15](F)[C:16]=3[Cl:18])[C:11](=[O:21])[C:10]([C:22]([OH:24])=[O:23])=[CH:9]2)[CH:7]=1.[CH2:27]([NH2:30])[CH2:28][NH2:29].C(N(CC)CC)C>C(#N)C>[NH2:29][CH2:28][CH2:27][NH:30][C:15]1[C:16]([Cl:18])=[C:17]2[C:12]([C:11](=[O:21])[C:10]([C:22]([OH:24])=[O:23])=[CH:9][N:8]2[C:6]2[CH:7]=[C:2]([NH2:1])[C:3]([F:26])=[CH:4][C:5]=2[F:25])=[CH:13][C:14]=1[F:20]

参加物

5

反応物 3

HCID 3301EthylenediamineHCID 8471TriethylamineHCID 108619991-(3-Amino-4,6-difluorophenyl)-8-chloro-6,7-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

生成物 1

HCID 232848167-(2-Aminoethyl)amino-1-(5-amino-2,4-difluorophenyl)-8-chloro-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid収率 65.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

1-(5-Amino-2,4-difluorophenyl)-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (100 mg), ethylenediamine (16 mg) and triethylamine (70 mg) were added to acetonitrile (5 ml), and the mixture was heated under reflux for 2 hours. After the reaction mixture was allowed to cool, deposits were collected by filtration. The deposits were washed successively with ethanol and diethyl ether to obtain the title compound (72 mg) as a pale yellow powder.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. temperatureto cool
  4. filtrationdeposits were collected by filtration
  5. washThe deposits were washed successively with ethanol and diethyl ether

出典と根拠

ORDレコード
ord-8c051533994245df9eca183ed04e9055
出典データセット
uspto-grants-2000_10
特許番号
US06136823

反応ノート

読み込み中…