Sodium Hydroxide → 8-Fluoro-1-methyl-4-oxo-1,4-dihydroquinol-3-yl methanesulphonate

HRID 358675ノート

反応式

HRID 358675 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[F:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]([CH3:17])[CH:14]=[C:13]([OH:18])[C:12]2=[O:19].[OH-].[Na+]>O>[CH3:1][S:2]([O:18][C:13]1[C:12](=[O:19])[C:11]2[C:16](=[C:7]([F:6])[CH:8]=[CH:9][CH:10]=2)[N:15]([CH3:17])[CH:14]=1)(=[O:4])=[O:3]

参加物

5

反応物 3

HCID 14798Sodium Hydroxide3 回HCID 31297Methanesulfonyl chloride2 回HCID 231281098-Fluoro-3-hydroxy-1-methyl-4-quinolone

生成物 1

HCID 537406098-Fluoro-1-methyl-4-oxo-1,4-dihydroquinol-3-yl methanesulphonate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Methanesulphonyl chloride (1.1 g) d to a solution of 8-fluoro-3-hydroxy-1 -methyl-4-quinolone (1.83 g) and sodium hydroxide (0.6 g) in water (15 ml) and the resultant mixture stirred at 0 to 5° for 3 hours with the pH being adjusted to 9 after 20 minutes using aqueous sodium hydroxide (5M, 2 ml). Further methanesulphonyl chloride (1.1 g) was then added and the mixture stirred for 105 minutes whilst maintaining the pH at 9 by the addition of aqueous sodium hydroxide (5M, 2ml). The resultant solid was collected by filtration, washed with water (20 ml) and crystallised from industrial methylated spirit (100 ml) to give the novel compound 8-fluoro-1-methyl-4-oxo-1,4-dihydroquinol-3-yl methanesulphonate, m.p. 207°-209°.

後処理

  1. temperaturewhilst maintaining the pH at 9
  2. filtrationThe resultant solid was collected by filtration
  3. washwashed with water (20 ml)
  4. customcrystallised from industrial methylated spirit (100 ml)

出典と根拠

ORDレコード
ord-5899096f2b07466f8aa64790839cd599
出典データセット
uspto-grants-1991_03
特許番号
US04997840

反応ノート

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