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

HRID 378581

反応式

HRID 378581 の反応式
[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

参加物

7

反応物 4

HCID 240BenzaldehydeHCID 313Hydrochloric AcidHCID 7294Methyl AcrylateHCID 9237Dabco

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3cb3d5c663e44fe8a5662d593968671b
出典データセット
uspto-grants-2000_02
特許番号
US06031121

関連ノート

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