Hydrochloric Acid → 4-Phenoxy-2-butanol

HRID 580107ノート

反応式

HRID 580107 の反応式
[O:1]([CH2:8][CH2:9][CH:10]=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:12][Mg]I.Cl>C(OCC)C>[O:1]([CH2:8][CH2:9][CH:10]([OH:11])[CH3:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

実験手順

24.9 g of methyl iodide was reacted with 7.26 g of magnesium in 150 ml of anhydrous diethyl ether to obtain methylmagnesium iodide by Grignard reaction. To a solution consisting of 20 g of 3-phenoxypropionaldehyde and 200 ml of anhydrous diethyl ether was added dropwise the methylmagnesium while maintaining a temperature of not more than 20° C. The reaction solution was added with 25 ml of concentrated hydrochloric acid, and then the diethyl ether layer was separated from an aqueous layer. The ether layer was washed with an aqueous sodium bicarbonate solution, washed with water, dried over anhydrous sodium sulfate and then condensed under reduced pressure to obtain 15.0 g of 4-phenoxy-2-butanol having a boiling point of 61° C. to 62° C. at 3 mmHg in a yield of 67%.

後処理

  1. customby Grignard reaction
  2. temperaturewhile maintaining a temperature of not more than 20° C
  3. customthe diethyl ether layer was separated from an aqueous layer
  4. washThe ether layer was washed with an aqueous sodium bicarbonate solution
  5. washwashed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customcondensed under reduced pressure

出典と根拠

ORDレコード
ord-28fbe674a30646ebb20133e4e952f62e
出典データセット
uspto-grants-1988_06
特許番号
US04751302

反応ノート

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