Hydrochloric Acid → Benzyl 2-benzyloxy-4-hydroxybenzoate

HRID 2220601노트

반응식

HRID 2220601 반응식
[OH-].[Na+].C([O:11][C:12]1[CH:27]=[CH:26][C:15]([C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])=[C:14]([O:28][CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH:13]=1)(=O)C1C=CC=CC=1.Cl>CO>[CH2:29]([O:28][C:14]1[CH:13]=[C:12]([OH:11])[CH:27]=[CH:26][C:15]=1[C:16]([O:18][CH2:19][C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)=[O:17])[C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 23090801Benzyl 4-benzoyloxy-2-benzyloxybenzoate

생성물 1

HCID 23090785Benzyl 2-benzyloxy-4-hydroxybenzoate수율 40.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A 2 mol/L aqueous solution of sodium hydroxide (6.39 mL) was added to a mixture of benzyl 4-benzoyloxy-2-benzyloxybenzoate (2.80 g) in methanol/tetrahydorofuran (1/1, 20 mL), and the mixture was stirred at room temperature for 5 hrs. To the reaction mixture was added 2 mol/L hydrochloric acid (6.39 mL). The solvent was evaporated under reduced pressure, and water was added to the residue. The resulting mixture was extracted with ethyl acetate. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by medium-pressure silica gel column chromatography (eluent: n-hexane/ethyl acetate=4/1) to afford benzyl 2-benzyloxy-4-hydroxybenzoate (0.859 g)

후처리

  1. customThe solvent was evaporated under reduced pressure, and water
  2. additionwas added to the residue
  3. extractionThe resulting mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was purified by medium-pressure silica gel column chromatography (eluent: n-hexane/ethyl acetate=4/1)

출처 및 근거

ORD 기록
ord-a52ca05c3c6549e48e0dfeccc4ed3274
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07417169B2

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