Benzyl Bromide → Benzyl 4-hydroxybutanoate

HRID 1648199

반응식

HRID 1648199 반응식
[OH:1][CH2:2][CH2:3][CH2:4][C:5]([O-:7])=[O:6].[Na+].[CH2:9](Br)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>CN(C=O)C.C(OCC)(=O)C>[OH:1][CH2:2][CH2:3][CH2:4][C:5]([O:7][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:6]

참가 물질

5

반응물 2

HCID 7498Benzyl BromideHCID 23663870Sodium Oxybate

생성물 1

HCID 14443958Benzyl 4-hydroxybutanoate수율 90%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매2회

실험 절차

Sodium 4-hydroxybutyrate (25 g, 0.2 mol) and benzyl bromide (37 g, 0.22 mol) were dissolved in a mixed solvent of DMF (40 ml) and ethyl acetate (50 ml), and the reaction mixture was heated and refluxed for 4 hours. Then, the reaction mixture was allowed to cool to room temperature, diluted with a proper amount of ethyl acetate, washed with saturated saline solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give an oily product. The resulted product was purified by silica gel column chromatography (eluent:hexane/ethyl acetate=4/1) to give 34.9 g of benzyl 4-hydroxybutyrate. Yield: 90%.

후처리

  1. temperaturethe reaction mixture was heated
  2. temperaturerefluxed for 4 hours
  3. washwashed with saturated saline solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give an oily product
  7. customThe resulted product was purified by silica gel column chromatography (eluent:hexane/ethyl acetate=4/1)

출처 및 근거

ORD 기록
ord-8589ef1ff6444beb9f10a15383b1c7f5
출처 데이터셋
uspto-grants-1995_07
특허 번호
US05436221

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