Norfloxacin → HCID 19812304、化合物

HRID 467275

反応式

HRID 467275 の反応式
[CH3:1][CH2:2][N:3]1[C:9]2[CH:10]=[C:11]([N:15]3[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]3)[C:12]([F:14])=[CH:13][C:8]=2[C:6](=[O:7])[C:5]([C:21]([OH:23])=[O:22])=[CH:4]1.Br[CH2:25][CH:26]1[CH2:31][CH2:30][N:29]([CH:32]=[O:33])[CH2:28][CH2:27]1.C(N(CC)CC)C>CN(C)C=O>[CH2:2]([N:3]1[C:9]2[C:8](=[CH:13][C:12]([F:14])=[C:11]([N:15]3[CH2:20][CH2:19][N:18]([CH2:25][CH:26]4[CH2:31][CH2:30][N:29]([CH:32]=[O:33])[CH2:28][CH2:27]4)[CH2:17][CH2:16]3)[CH:10]=2)[C:6](=[O:7])[C:5]([C:21]([OH:23])=[O:22])=[CH:4]1)[CH3:1]

参加物

5

反応物 3

HCID 4539NorfloxacinHCID 8471TriethylamineHCID 19812293N-Formyl-4-bromomethylpiperidine

生成物 1

HCID 19812304HCID 19812304、化合物収率 75%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

A mixture of norfloxacin (0.96 g, 3 mmol), 4-bromomethyl-1-formylpiperidine (1.26 g, 6.1 mmol) and triethylamine (0.44 g, 0.6 mL, 4.3 mmol) in anhydrous dimethylformamide (15 mL) was heated at 100° C. for 2 hours. The solvent was removed under high vacuum and the residue was dissolved in methanol, filtered and precipitated by the addition of diethyl ether to give the product as a white solid (1.0 g, 75% yield).

後処理

  1. customThe solvent was removed under high vacuum
  2. dissolutionthe residue was dissolved in methanol
  3. filtrationfiltered
  4. customprecipitated by the addition of diethyl ether

出典と根拠

ORDレコード
ord-50a0ee4c0eca45e68746624c5755f8f6
出典データセット
uspto-grants-1992_10
特許番号
US05159077

関連ノート

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