Sodium Hydroxide → HCID 22388009、化合物

HRID 1072788ノート

反応式

HRID 1072788 の反応式
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

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22388180HCID 22388180、化合物

生成物 1

HCID 22388009HCID 22388009、化合物収率 27.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2bd9940ec2054ba198650e18f38eaaf0
出典データセット
uspto-grants-2005_06
特許番号
US06911469B2

反応ノート

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