FERROCENEACETIC ACID synthesis

Yield:1287-16-7 79%

Reaction Conditions:

Stage #1:acetylferrocene with morpholine;sodiumsulfide nonahydrate;sulfur at 128; for 7 h;
Stage #2: with sodium hydroxide in ethanol;water for 4 h;Reflux;Temperature;

Steps:

1.1 Preparation of ferrocenyl acetic acid:
To a 500 mL three-necked flask equipped with a mechanical stirrer and a spherical condenser were added 0.01 mol of acetyl ferrocene,0.1 mol morpholine,0.05 mol of sulfur and 0.001 mol of Na2S · 9H2O, Oil bath was heated to 128 deg C, Reflux 7h, TLC monitoring.The reaction is completed,The mixture was cooled to room temperature,Then, 10 mL of ethanol and 25 mL of 2 mol / L sodium hydroxide aqueous solution were added thereto,Stirring temperature,Reflux 4h,TLC monitoring.The reaction is completed,cool down,Adjust the pH value with hydrochloric acid to between 7 and 8,Filter cleaning,The filtrate was then adjusted to pH 1 with hydrochloric acid,Placed overnight,filter,Washed,A yellow-brown solid,Namely ferrocenyl acetic acid,The yield is 79%.

References:

Shaanxi University of Science and Technology;Liu, Yuting;Song, Simeng;Yin, Dawei;Jiang, Shanshan;Liu, Beibei;Yang, Aning;Wang, Jinyu;Lyu, Bo CN104231004, 2017, B Location in patent:Paragraph 0033; 0042; 0051; 0060; 0069

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