反応式
Cl.Cl.[OH:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.C(N(CC)CC)C.[CH2:17]([N:19]1[C:28]2[C:23](=[CH:24][C:25]([F:31])=[C:26](F)[C:27]=2[F:29])[C:22](=[O:32])[C:21]([C:33]([OH:35])=[O:34])=[CH:20]1)[CH3:18].Cl>O.CS(C)=O>[CH2:17]([N:19]1[C:28]2[C:23](=[CH:24][C:25]([F:31])=[C:26]([N:7]3[CH2:8][CH2:9][N:4]([OH:3])[CH2:5][CH2:6]3)[C:27]=2[F:29])[C:22](=[O:32])[C:21]([C:33]([OH:35])=[O:34])=[CH:20]1)[CH3:18]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 100 °C
実験手順
1-Hydroxypiperazine dihydrochloride (3.94 g) (which is prepared in Preparation 1), triethylamine (21 ml) and dimethylsulfoxide (30 ml) are added to 1-ethyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (4.07 g), which is prepared according to the procedure described in Japanese Patent First Publication No. 30964/1981, and the mixture is heated at 100° C. for 30 minutes. After cooling to room temperature, water (200 ml) is added to the mixture and the pH is adjusted to 7.0 with dil. HCl. The precipitated crystals are filtered, washed with water and dried. The product is recrystallized from a mixture of dimethylformamide and water to yield 1-ethyl-6,8-difluoro-1,4-dihydro-7-(4-hydroxypiperazin-1-yl)-4-oxoquinoline-3-carboxylic acid (4.3 g) as pale yellow needles, m.p. 253°-260° C. (decomposed with foaming) (which starts to color brown at around 234° C.).
後処理
- customis prepared
- temperatureAfter cooling to room temperature
- filtrationThe precipitated crystals are filtered
- washwashed with water
- customdried
- customThe product is recrystallized from a mixture of dimethylformamide and water
出典と根拠
- ORDレコード
- ord-69a2a105fbf243efb1c35a56bb089878
- 出典データセット
- uspto-grants-1987_08
- 特許番号
- US04686221
関連ノート
読み込み中…