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Methane → 1-Ethyl-6,8-difluoro-1,4-dihydro-4-oxo-7-[3-(4-acetamidobenzenesulfonamido)-1-pyrrolidinyl]-3-quinolinecarboxylic acid

HRID 1290734
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HRID 1290734 반응식
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:20])=[C:10]([N:14]3[CH2:18][CH2:17][CH:16]([NH2:19])[CH2:15]3)[C:11]=2[F:13])[C:6](=[O:21])[C:5]([C:22]([OH:24])=[O:23])=[CH:4]1)[CH3:2].[C:25]([NH:28][C:29]1[CH:34]=[CH:33][C:32]([S:35](Cl)(=[O:37])=[O:36])=[CH:31][CH:30]=1)(=[O:27])[CH3:26].C>N1C=CC=CC=1.C1C=CC=CC=1.CN(C)C=O>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:20])=[C:10]([N:14]3[CH2:18][CH2:17][CH:16]([NH:19][S:35]([C:32]4[CH:31]=[CH:30][C:29]([NH:28][C:25](=[O:27])[CH3:26])=[CH:34][CH:33]=4)(=[O:37])=[O:36])[CH2:15]3)[C:11]=2[F:13])[C:6](=[O:21])[C:5]([C:22]([OH:24])=[O:23])=[CH:4]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 297MethaneHCID 8481N-Acetylsulfanilyl chlorideHCID 11724607HCID 11724607, 화합물

생성물 1

HCID 189182031-Ethyl-6,8-difluoro-1,4-dihydro-4-oxo-7-[3-(4-acetamidobenzenesulfonamido)-1-pyrrolidinyl]-3-quinolinecarboxylic acid수율 32.7%

시약·촉매·용매 3

HCID 241Benzene용매
HCID 1049
Pyridine
용매
HCID 6228Dimethylformamide용매

실험 절차

2.80 g of 1-ethyl-6,8-difluoro-1,4-dihydro-4-oxo-7-(3-amino-1-pyrrolidinyl)-3-quinolinecarboxylic acid (see REFERENCE SYNTHESIS EXAMPLE hereinafter) is suspended in 100 ml of pyridine. To this is slowly added 3.88 g of 4-acetamidobenzenesulfonyl chloride in 20 ml of benzene. The mixture is stirred for 1 hour under ice-cooling and then overnight at room temperature. After evaporating off the solvent from the reaction mixture, the residue is added water and then adjusted to pH 12 with 2N sodium hydroxide solution. Any undissolved matter, if present, is filtered off. The filtrate is adjusted to pH 7 with acetic acid. The precipitated crystals are collected by filtration and washed. The crystals are then suspended in 100 ml of water. The suspension is adjusted to pH 4 with acetic acid, stirred and then filtered to recover the crystals, which are then thoroughly washed with water. The crude crystals thus obtained are dissolved in dimethylformamide (DMF), treated with activated charcoal, and recrystallized from DMF-methanol to give 1.45 g of the titled compound.

후처리

  1. temperaturecooling
  2. customovernight
  3. customat room temperature
  4. customAfter evaporating off the solvent from the reaction mixture
  5. additionthe residue is added water
  6. filtrationAny undissolved matter, if present, is filtered off
  7. filtrationThe precipitated crystals are collected by filtration
  8. washwashed
  9. stirringstirred
  10. filtrationfiltered
  11. customto recover the crystals, which
  12. washare then thoroughly washed with water
  13. customThe crude crystals thus obtained
  14. customrecrystallized from DMF-methanol

출처 및 근거

ORD 기록
ord-00ecf782a6eb4c62b73d4b91c84051fe
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753658

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