反応 #57398

反応方程式

heptane

N-[2,3,6-trimethyl-4-[[2-methyl-3-(4-methylphenyl)-2-propenyl]oxy]phenyl]formamide

potassium carbonate

N,N-dimethylaniline

heptane

→

title compound

収率 86.9%

N-[4-hydroxy-3-[2-methyl-1-(4-methylphenyl)-1-propenyl]-2,5,6-trimethylphenyl]formamide

収率 86.9%

反応条件

後処理

1. 1
   温度The mixture was cooled to 100° C.
2. 2
   温度The mixture was further cooled to 30° C.
3. 3
   workup.STIRRINGThe mixture was stirred at the same temperature for 1 hr
4. 4
   ろ過the precipitated crystals were collected by filtration
5. 5
   洗浄washed with heptane

実験手順

A mixture of N-[2,3,6-trimethyl-4-[[2-methyl-3-(4-methylphenyl)-2-propenyl]oxy]phenyl]formamide (920 g), potassium carbonate (4.6 g) and N,N-dimethylaniline (2760 ml) was stirred at 190° C. for 4 hr under nitrogen stream. The mixture was cooled to 100° C. and heptane (1840 ml) was added dropwise thereto. The mixture was further cooled to 30° C. and heptane (3680 ml) was added dropwise thereto. The mixture was stirred at the same temperature for 1 hr, and the precipitated crystals were collected by filtration and washed with heptane to give the title compound (799.5 g, yield 86.9%).

出典