3-苯基丙-1-烯-2-醇

反应条件: temp:78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a 2 liter reaction flask equipped with stirrer, thermometer, reflux condenser, heating mantle and Bidwell addition funnel is placed 222 grams of dimethyl carbonate and 24 grams of a solution of sodium methoxide in methanol. The resulting mixture is heated to reflux. Over a 30 minute period 268 grams of alpha-methylene phenylethyl alcohol having the structure: ##STR161## is added over a period of 20 minutes after bringing the mixture to reflux at 72°-76° C. At the end of the addition of the alpha-methylene phenylethyl alcohol the reaction mass is continued to be refluxed at 78° C. for a period of two hours. At the end of the two hour period, the excess methyl alcohol is taken off at 100° C. The reaction mass is then cooled and 200 ml wter is added thereto. The organic phase is then distilled on a 12" Goodloe column yielding the following fractions: Into a 2 liter reaction flask equipped with stirrer thermometer, reflux condenser heating mantle Bidwell addition funnel The resulting mixture is heated to reflux ##STR161## is added over a period of 20 minutes to reflux at 72°-76° C At the end of the two hour period is taken off at 100° C The reaction mass is then cooled 200 ml wter is added The organic phase is then distilled on a 12" Goodloe column yielding the following fractions

反应条件: temp:78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a 2 liter reaction flask equipped with stirrer, thermometer, reflux condenser, heating mantle and Bidwell addition funnel is placed 222 grams of dimethyl carbonate and 24 grams of a solution of sodium methoxide in methanol. The resulting mixture is heated to reflux. Over a 30 minute period 268 grams of alpha-methylene phenylethyl alcohol having the structure: ##STR161## is added over a period of 20 minutes after bringing the mixture to reflux at 72°-76° C. At the end of the addition of the alpha-methylene phenylethyl alcohol the reaction mass is continued to be refluxed at 78° C. for a period of two hours. At the end of the two hour period, the excess methyl alcohol is taken off at 100° C. The reaction mass is then cooled and 200 ml wter is added thereto. The organic phase is then distilled on a 12" Goodloe column yielding the following fractions: Into a 2 liter reaction flask equipped with stirrer thermometer, reflux condenser heating mantle Bidwell addition funnel The resulting mixture is heated to reflux ##STR161## is added over a period of 20 minutes to reflux at 72°-76° C At the end of the two hour period is taken off at 100° C The reaction mass is then cooled 200 ml wter is added The organic phase is then distilled on a 12" Goodloe column yielding the following fractions