Hydrochloric Acid → 2-(2-Benzyloxy-5-nitrophenyl)-2-methylpropionic acid

HRID 1861968노트

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HRID 1861968 반응식
C[O:2][C:3](=[O:24])[C:4]([C:7]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[CH:9][C:8]=1[O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([CH3:6])[CH3:5].[OH-].[Li+].Cl.C(OCC)(=O)C>O1CCOCC1>[CH2:17]([O:16][C:8]1[CH:9]=[CH:10][C:11]([N+:13]([O-:15])=[O:14])=[CH:12][C:7]=1[C:4]([CH3:6])([CH3:5])[C:3]([OH:24])=[O:2])[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8857Ethyl AcetateHCID 229809592-(2-Benzyloxy-5-nitrophenyl)-2-methylpropionic acid methyl ester

생성물 1

HCID 186221532-(2-Benzyloxy-5-nitrophenyl)-2-methylpropionic acid수율 92%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

To the compound (1.54 g) obtained in Example 562 in 1, 4-dioxane (20 ml) was added an aqueous lithium hydroxide solution (1.0M, 47 ml). The reaction mixture was heated under reflux at 100° C. for 12 h and then 2 N HCl and ethyl acetate were added. The organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was recrystallized from ethyl acetate to give 1.355 g of the titled compound (yield, 92%).

후처리

  1. temperatureThe reaction mixture was heated
  2. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resulting residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-b9a3596ee8c545d08528e60a7d260177
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06534546B1

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