反応式
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:15])=[C:10](F)[C:11]=2[F:13])[C:6](=[O:16])[C:5]([C:17]([OH:19])=[O:18])=[CH:4]1)[CH3:2].Cl.[CH:21]([NH:23][CH2:24][CH:25]1[O:30][CH2:29][CH2:28][NH:27][CH2:26]1)=[O:22].N12CCCN=C1CCCCC2>C(#N)C>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:15])=[C:10]([N:27]3[CH2:28][CH2:29][O:30][CH:25]([CH2:24][NH:23][CH:21]=[O:22])[CH2:26]3)[C:11]=2[F:13])[C:6](=[O:16])[C:5]([C:17]([OH:19])=[O:18])=[CH:4]1)[CH3:2]参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of 813 mg of 1-ethyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 650 mg of 2-(formylaminomethyl)morpholine hydrochloride and 1.0 g of 1,8-diazabicyclo[5.4.0]undec-7-ene in 10 ml of acetonitrile is refluxed for 3 hours and allowed to stand at room temperature overnight. The precipitated crystals are collected by filtration and successively washed with acetonitrile, water and acetone to give 1-ethyl-6,8-difluoro-7-[2-(formylaminomethyl)morpholino]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, melting at 234°-236° C.
後処理
- filtrationThe precipitated crystals are collected by filtration
- washsuccessively washed with acetonitrile, water and acetone
出典と根拠
- ORDレコード
- ord-86916008a3a74584aa92e85bdd727e74
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04889857
関連ノート
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