DIETHYL ISOBUTYLIDENEMALONATE synthesis

4synthesis methods

Product Name:DIETHYL ISOBUTYLIDENEMALONATE
CAS Number:5652-68-6
Molecular formula:C11H18O4
Molecular Weight:214.26

78-84-2
371 suppliers
$10.00/25mL

105-53-3
746 suppliers
$5.00/25g

5652-68-6
26 suppliers
$60.00/100mg

Yield:5652-68-6 93%

Reaction Conditions:

with piperidine;glacial acetic acid in benzene; for 3 h;Dean-Stark;Reflux;

Steps:

Synthesis of alkylidenemalonates 3a and 3b

General procedure: A solution of 8 g (0.1 mol) of aldehyde 2a or 2b, 16 g(0.1 mol) of diethyl malonate 1, 0.85 g (0.01 mol) of piperidine, and 1.2 g (0.02 mol) of acetic acid in 40 mLof C6H6 was heated at reflux with a Dean-Stark trap for 3 h until water evolution ceased. The resultant mixture was cooled and washed with water until the pH in the solution became neutral, dried with Na2SO4, the solvent was removed by rotary evaporation to give 20 gof diethyl butylidenemalonate (3a) (yield 95%), bp101°C (6 mmHg) and 19.7 g of diethyl (2-methylpropylidene)malonate (3b) (yield 93%), bp 106°C(6 mmHg)

References:

Borisova, Yu. G.;Raskil’dina;Zlotskii [Doklady Chemistry,2017,vol. 476,# 1,p. 201 - 205][Dokl. Akad. Nauk,2017,vol. 476,# 1,p. 39 - 44,6]