Sodium Hydroxide → Magnesium [5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate]

HRID 1440121노트

반응식

HRID 1440121 반응식
[OH-].[Na+].[NH2:3][C:4]1[C:13]([F:14])=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:11]([O:22][CH:23]([F:25])[F:24])=[C:10]2[C:5]=1[C:6](=[O:32])[C:7]([C:29]([OH:31])=[O:30])=[CH:8][N:9]2[CH:26]1[CH2:28][CH2:27]1.[Cl-].[Mg+2:34].[Cl-]>>[NH2:3][C:4]1[C:13]([F:14])=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:11]([O:22][CH:23]([F:24])[F:25])=[C:10]2[C:5]=1[C:6](=[O:32])[C:7]([C:29]([O-:31])=[O:30])=[CH:8][N:9]2[CH:26]1[CH2:27][CH2:28]1.[Mg+2:34].[NH2:3][C:4]1[C:13]([F:14])=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:11]([O:22][CH:23]([F:24])[F:25])=[C:10]2[C:5]=1[C:6](=[O:32])[C:7]([C:29]([O-:31])=[O:30])=[CH:8][N:9]2[CH:26]1[CH2:27][CH2:28]1

참가 물질

4

반응물 3

HCID 14798Sodium HydroxideHCID 5360315Magnesium ChlorideHCID 150238035-Amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

생성물 1

HCID 21619245Magnesium [5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate]수율 90.4%

실험 절차

23.0 ml (0.0023 mole) of a 0.1N aqueous solution of sodium hydroxide were added to 1.00 g (0.00234 mole) of 5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (prepared as described in Example 30), and the resulting insoluble material was removed by filtration. 0.11 g (0.00115 mole) of anhydrous magnesium chloride was added to the filtrate, and the mixture was stirred at room temperature for 90 minutes. At the end of this time, the resulting precipitate was collected by filtration and washed with water, to give 0.91 g of magnesium [5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate] as a yellow powder, melting at 291°-293° C. (with decomposition).

후처리

  1. customthe resulting insoluble material was removed by filtration
  2. filtrationAt the end of this time, the resulting precipitate was collected by filtration
  3. washwashed with water

출처 및 근거

ORD 기록
ord-8b7358fe8c3545a9b74de81ac4ba56a3
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05496951

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