Ethyl 3-hydroxy-3-(4-methoxyphenyl)-2-methylpropanoate → Ethyl 3-(4-methoxyphenyl)-2-methylprop-2-enoate

HRID 461095ノート

反応式

HRID 461095 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9](O)[CH:10]([CH3:16])[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:5][CH:4]=1.S([O-])(O)(=O)=O.[K+]>C1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH:9]=[C:10]([CH3:16])[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 312882Ethyl 3-hydroxy-3-(4-methoxyphenyl)-2-methylpropanoateHCID 516920Potassium bisulfate

生成物 1

HCID 53711494Ethyl 3-(4-methoxyphenyl)-2-methylprop-2-enoate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 71.8 g (0.30 mole) of ethyl β-(p-methoxyphenyl)-β-hydroxy-α-methylpropionate is refluxed with 41.0 g (0.30 mole) of potassium hydrogen sulfate in 718 ml of benzene for 1 hour. The insoluble white crystals formed are filtered off, washed with benzene and the solvent of the filtrate is removed on evaporation. This is dissolved in 700 ml of ether. The ether solution is washed with 4 × 100 ml of cold water until neutral followed by 80 ml of saturated sodium chloride solution, then it is dried over magnesium sulfate for 1.5 hours and filtered. The solvent is removed on an evaporator to give ethyl p-methoxy-α-methylcinnamate.

後処理

  1. customThe insoluble white crystals formed
  2. filtrationare filtered off
  3. washwashed with benzene
  4. customthe solvent of the filtrate is removed on evaporation
  5. dissolutionThis is dissolved in 700 ml of ether
  6. washThe ether solution is washed with 4 × 100 ml of cold water
  7. dry with materialit is dried over magnesium sulfate for 1.5 hours
  8. filtrationfiltered
  9. customThe solvent is removed on an evaporator

出典と根拠

ORDレコード
ord-39daad5a7252463c95e3a8965db6eb2c
出典データセット
uspto-grants-1977_12
特許番号
US04061771

反応ノート

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