Benzyl Chloride → HCID 12944896, 화합물

HRID 544224노트

반응식

HRID 544224 반응식
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([Cl:19])=[C:10]([N:13]3[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[CH:11]=2)[C:6](=[O:20])[C:5]([C:21]([OH:23])=[O:22])=[CH:4]1)[CH3:2].[CH2:24](Cl)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C(N(CC)CC)C>CN(C=O)C>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([Cl:19])=[C:10]([N:13]3[CH2:18][CH2:17][N:16]([CH2:24][C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)[CH2:15][CH2:14]3)[CH:11]=2)[C:6](=[O:20])[C:5]([C:21]([OH:23])=[O:22])=[CH:4]1)[CH3:2]

참가 물질

5

반응물 3

HCID 7503Benzyl ChlorideHCID 8471TriethylamineHCID 30516953-Quinolinecarboxylic acid, 1,4-dihydro-6-chloro-1-ethyl-4-oxo-7-(1-piperazinyl)-

생성물 1

HCID 12944896HCID 12944896, 화합물수율 52%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1-ethyl-6-chloro-7-(1-piperazinyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid 1.7 g (0.005 mole), benzylchloride 1.26 g (0.01 mole), triethylamine (0.01 mole) and DMF 10 ml was heated at 90°-100° C. for 7 hours under stirring. After cooling, the reaction mixture was dried up under vacuum. The residue was dissolved in CHCl3, washed with water, dried with anhydrous Na2SO4, and the solvent was distilled off. The residue was recrystallized from a mixed solvent of DMF and ethanol to obtain 1.1 g (52%) of 1-ethyl-6-chloro-7-(4-benzyl-1-piperazinyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid. Colorless prism.

후처리

  1. temperaturewas heated at 90°-100° C. for 7 hours
  2. temperatureAfter cooling
  3. customthe reaction mixture was dried up under vacuum
  4. dissolutionThe residue was dissolved in CHCl3
  5. washwashed with water
  6. dry with materialdried with anhydrous Na2SO4
  7. distillationthe solvent was distilled off
  8. customThe residue was recrystallized from a mixed solvent of DMF and ethanol

출처 및 근거

ORD 기록
ord-4a5592b80f9f4441b6a73b05c0f4f08b
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04448962

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