Sodium Hydroxide → 1-Ethyl-6-fluoro-7-[3-(fluoromethyl)-4-methyl-1-piperazinyl]-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

HRID 2165621노트

반응식

HRID 2165621 반응식
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:21])=[C:10]([N:13]3[CH2:18][CH2:17][NH:16][CH:15]([CH2:19][F:20])[CH2:14]3)[CH:11]=2)[C:6](=[O:22])[C:5]([C:23]([OH:25])=[O:24])=[CH:4]1)[CH3:2].[CH:26]([O-])=O.[Na+].[OH-].[Na+]>C(O)(=O)C.C=O>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:21])=[C:10]([N:13]3[CH2:18][CH2:17][N:16]([CH3:26])[CH:15]([CH2:19][F:20])[CH2:14]3)[CH:11]=2)[C:6](=[O:22])[C:5]([C:23]([OH:25])=[O:24])=[CH:4]1)[CH3:2]

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 2723810Sodium FormateHCID 14839365HCID 14839365, 화합물

생성물 1

HCID 148393661-Ethyl-6-fluoro-7-[3-(fluoromethyl)-4-methyl-1-piperazinyl]-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 712Formaldehyde용매

실험 절차

A 100 mg portion of 1-ethyl-6-fluoro-7-[3-(fluoromethyl)-1-piperazinyl]-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid and 300 mg of sodium formate were dissolved in a mixture of 3 ml of glacial acetic acid and 3 ml of 37% formaldehyde and refluxed overnight. The mixture was cooled, basified with sodium hydroxide, acidified with glacial acetic acid and evaporated. The residue was triturated with hot chloroform and the solid crystallized from methanol, giving 91 mg of the desired product, mp 230°-235° C. (dec.).

후처리

  1. temperaturerefluxed overnight
  2. temperatureThe mixture was cooled
  3. customevaporated
  4. customThe residue was triturated with hot chloroform
  5. customthe solid crystallized from methanol

출처 및 근거

ORD 기록
ord-b8cff32e3ef74524b4822880ff60b3b5
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04940710

반응 노트

불러오는 중…