Sodium Hydroxide → HCID 22388009, 화합물

HRID 1699807노트

반응식

HRID 1699807 반응식
C(OC([N:6]1[C:15]2[C:10](=[CH:11][C:12]([C:16]3[O:17][CH2:18][C:19]([CH3:22])([CH3:21])[N:20]=3)=[CH:13][CH:14]=2)[C:9]([CH2:23][C:24]2[CH:29]=[CH:28][C:27]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)=[CH:26][CH:25]=2)=[CH:8][CH:7]1P(OC)(OC)=O)=O)C.[OH-].[Na+]>C(O)C>[CH3:21][C:19]1([CH3:22])[CH2:18][O:17][C:16]([C:12]2[CH:11]=[C:10]3[C:15](=[CH:14][CH:13]=2)[N:6]=[CH:7][CH:8]=[C:9]3[CH2:23][C:24]2[CH:29]=[CH:28][C:27]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)=[CH:26][CH:25]=2)=[N:20]1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22388180HCID 22388180, 화합물

생성물 1

HCID 22388009HCID 22388009, 화합물수율 27.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1-ethoxycarbonyl-6-(4,5-dihydro-4,4-dimethyloxazol-2-yl)-2-dimethoxyphosphoryl-4-(4-phenylbenzyl)-1,2-dihydroquinoline (738 mg), ethanol (20 ml) and 1N aqueous sodium hydroxide solution (4 ml) was refluxed under heating for 2 hr. The reaction mixture was concentrated to dryness under reduced pressure. Water was added and the mixture was extracted twice with ethyl acetate. The organic layers were combined, washed once with saturated brine, dried over anhydrous magnesium sulfate and concentrated to dryness under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate) to give the objective compound (140 mg) as a white solid.

후처리

  1. temperaturewas refluxed
  2. temperatureunder heating for 2 hr
  3. concentrationThe reaction mixture was concentrated to dryness under reduced pressure
  4. additionWater was added
  5. extractionthe mixture was extracted twice with ethyl acetate
  6. washwashed once with saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated to dryness under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate)

출처 및 근거

ORD 기록
ord-8ea46165533745b6b65cbc63ad92f143
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06348474B1

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