Water → Benzyl 2-bromo-5-nitrobenzoate

HRID 2103750노트

반응식

HRID 2103750 반응식
[Br:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C.C(Br)C1C=CC=CC=1>[CH2:4]([O:5][C:4](=[O:6])[C:3]1[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:2]=1[Br:1])[C:3]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:2]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 2430252-Bromo-5-nitrobenzoic acid

생성물 1

HCID 19038758Benzyl 2-bromo-5-nitrobenzoate수율 187.7%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 7498Benzyl Bromide용매

실험 절차

Under an atmosphere of argon, to a solution of 2-bromo-5-nitrobenzoic acid (5.14 g) in DMF, benzyl bromide (2.73 mL) and potassium carbonate (4.33 g) were added. The mixture was stirred for 30 minutes at room temperature. To the reaction mixture, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride, dried over magnesium sulfate and concentrated. The residue was washed with hexane/ethyl acetate to give the title compound (6.59 g) having the following physical data.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materiala saturated aqueous solution of sodium chloride, dried over magnesium sulfate
  4. concentrationconcentrated
  5. washThe residue was washed with hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-096c688eeb30442b9eadb70c82d7af4a
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576129B2

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