2-Propen-1-one, 3-[4-(1,1-dimethylethyl)phenyl]-1-(4-methoxyphenyl)- synthesis

Yield:258497-50-6 94.6%

Reaction Conditions:

with sodium hydroxide in methanol at 25; for 4 h;

Steps:

1.1; 1.2

(1) 150.2 g (1.0 mol) of p-methoxyacetophenone and200g (6.25mol) methanol solution to be used,In a dry, with a stirrer, thermometer,Constant pressure dropping funnel and condenser tube 2000mL four-necked flask,Add 800g (25.0mol) methanol, turn on stirring,At 25 ° C, 3.1 g (0.078 mol)Of solid sodium hydroxide,After stirring to dissolve, 162.2 g (1.0 mol) of p-tert-butylbenzaldehyde was added,The reaction temperature was controlled at 25 ,Slowly dropwise within 2.5h p-methoxy acetophenone in methanol,Dropping process, the gradual precipitation of crystals,A large number of crystals precipitated later.Dropping is completed, continue to heat the reaction 1.5h;
(2) Adjust pH = 6.5-7 with 4.77 g (0.08 mol) of acetic acid,Cold to 0 ~ 5 , filtered,The filter cake was washed with 100 g (3.12 mol)Cold methanol (5 ) wash,Filter cake at -0.1MPa, 70 drying 10h,Condensates to give 3 - ((4-t-butyl) phenyl) -1- (4-methoxyphenyl) -2-propen-1-one 278.5g,HPLC purity 99.57%, yield 94.6% (p-tert-butyl benzaldehyde).

References:

CN105085223,2017,B Location in patent:Paragraph 0032; 0106; 0107; 0111; 0112; 0116-0117; 0121-0122