Benzaldehyde → Methyl 3-Hydroxy-2-methylene-3-phenylpropionate

HRID 378581

반응식

HRID 378581 반응식
[CH:1](=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:9]([O:13][CH3:14])(=[O:12])[CH:10]=[CH2:11].N12CCN(CC1)CC2.Cl>C(OCC)(=O)C.O>[CH3:14][O:13][C:9](=[O:12])[C:10](=[CH2:11])[CH:1]([OH:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 240BenzaldehydeHCID 313Hydrochloric AcidHCID 7294Methyl AcrylateHCID 9237Dabco

생성물 1

HCID 9942369Methyl 3-Hydroxy-2-methylene-3-phenylpropionate

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of benzaldehyde (63.67 g; 600 mmol), methyl acrylate (60 ml; 667 mmol) and 1,4-diazabicyclo [2.2.2] octane (13.46 g; 120 mmol) is stirred at ambient temperature for 119 hours. To the reaction solution is added water (60 ml), 37% hydrochloric acid (60 ml) and ethyl acetate (120 ml), and then, the organic phase is extracted. The resulting organic phase is washed twice with saturated saline (60 ml), dried over anhydrous sodium sulfate and filtered, then concentrated under reduced pressure, to give a crude product of the title compound at a yield of 108.8 g.

후처리

  1. extractionthe organic phase is extracted
  2. washThe resulting organic phase is washed twice with saturated saline (60 ml)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3cb3d5c663e44fe8a5662d593968671b
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06031121

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