Nitric Acid → HCID 22980959, 화합물

HRID 1861967

반응식

HRID 1861967 반응식
S(=O)(=O)(O)O.[N+:6]([O-:9])(O)=[O:7].[CH3:10][O:11][C:12](=[O:30])[C:13]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[O:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)([CH3:15])[CH3:14].C(OCC)(=O)C>C(O)(=O)C>[CH3:10][O:11][C:12](=[O:30])[C:13]([C:16]1[CH:21]=[C:20]([N+:6]([O-:9])=[O:7])[CH:19]=[CH:18][C:17]=1[O:22][CH2:23][C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1)([CH3:15])[CH3:14]

참가 물질

6

반응물 4

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 8857Ethyl AcetateHCID 229809602-(2-Benzyloxyphenyl)-2-methylpropionic acid methyl ester

생성물 1

HCID 22980959HCID 22980959, 화합물수율 46%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
45 °C

실험 절차

To a mixture of sulfuric acid (0.27 ml) and nitric acid (0.34 ml), a solution of the compound (1.0 g) obtained in Example 561 in acetic acid (30 ml) was added dropwise at 5° C. The reaction mixture was stirred at 45° C. for 4 h, poured into ice cold water and ethyl acetate was added to the mixture. The organic layer was washed with a saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=9:1) to give 530 mg of the titled compound (yield, 46%).

후처리

  1. additionwas added to the mixture
  2. washThe organic layer was washed with a saturated aqueous sodium bicarbonate solution
  3. dry with materiala saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=9:1)

출처 및 근거

ORD 기록
ord-5268074992f94beda50fb17d68ce791d
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06534546B1

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