Hydrochloric Acid → 4-Phenoxy-2-butanol

HRID 464807ノート

反応式

HRID 464807 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

反応物 3

HCID 313Hydrochloric AcidHCID 109864123-PhenoxypropanalHCID 178418373HCID 178418373、化合物

生成物 1

HCID 113787034-Phenoxy-2-butanol収率 67%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

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. To the reaction solution was added 25 ml of concentrated hydrochloric acid and the solution was separated into two phases, which phases were then separated from each other. The ether layer was washed with an aqueous sodium bicarbonate solution, washed with water, dried with 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 solution was separated into two phases, which phases
  4. customwere then separated from each other
  5. washThe ether layer was washed with an aqueous sodium bicarbonate solution
  6. washwashed with water
  7. dry with materialdried with anhydrous sodium sulfate
  8. customcondensed under reduced pressure

出典と根拠

ORDレコード
ord-b19edbceb76a45d7978f32107fbaf2d2
出典データセット
uspto-grants-1985_10
特許番号
US04549023

反応ノート

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