Ethanol → alpha-Vinylbenzyl alcohol

HRID 1983977

반응식

HRID 1983977 반응식
C([O:4][CH:5]([CH:12]=[CH2:13])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)(=O)C.[OH-].[Na+].C(O)C>COC1C=CC(O)=CC=1.O>[CH:12]([CH:5]([OH:4])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[CH2:13]

참가 물질

6

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 111277Benzenemethanol, alpha-ethenyl-, 1-acetate

생성물 1

HCID 92986alpha-Vinylbenzyl alcohol수율 95%

시약·촉매·용매 2

HCID 90154-Methoxyphenol촉매HCID 962Water용매2회

반응 조건

온도
65 °C

실험 절차

120 grams (0.6876 mol) of vinylbenzyl acetate, inhibited with 10 mg of MEHQ were added to a one liter 3-neck round bottom flask equipped with a condenser, mechanical stirrer and thermometer, followed by 50 grams (1.25 mol) of sodium hydroxide. 50 mL of water and 300 mL of ethanol were then added and the contents of the flask heated at reflux (65° C.) for 2 hours. After the mixture was allowed to cool to room temperature, water was added. The content of the flask was poured into a separatory funnel and extracted with chloroform several times. The chloroform extract was subsequently washed several times with water and dried over magnesium sulfate. Removal of the chloroform on the rotary evaporator afforded 83 grams of the vinylbenzyl alcohol product (95% yield). The purification was accomplished by vacuum distillation.

후처리

  1. additionwere added to a one liter 3-neck round bottom flask
  2. customequipped with a condenser, mechanical stirrer
  3. temperaturethe contents of the flask heated
  4. temperatureto cool to room temperature
  5. additionThe content of the flask was poured into a separatory funnel
  6. extractionextracted with chloroform several times
  7. extractionThe chloroform extract
  8. dry with materialdried over magnesium sulfate
  9. customRemoval of the chloroform
  10. customon the rotary evaporator

출처 및 근거

ORD 기록
ord-4c66511c7ff14b63905c91ffc415ca9e
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544453B2

연결된 노트

불러오는 중…