Yield:6148-64-7 92%

Reaction Conditions:

with potassium hydroxide in ethanol at 20;Reflux;

Steps:

6.1
Step 1 - Ethyl potassium malonateA 2 litre round bottomed flask was charged with diethyl malonate (100g, 0.625 mol) and ethanol (400 ml) with magnetic agitation. A solution of KOH (35 g, 0.624 mol) in ethanol (400 ml) was added dropwise at room temperature and the mixture was stirred overnight, then the mixture was heated to reflux and allowed cool slowly to room temperature. A 1 ^st crop of the product was isolated by vacuum filtration through a large size 2 sintered glass funnel and left to dry for 1 hour. The mother liquor was reduced to 500 ml and allowed to cool to room temperature and a 2^nd crop of crystals was isolated; total 97.7g, 92%.

References:

PFIZER MANUFACTURING IRELAND;BURRELL, Adam James Musgrave;MARTINEZ, Carlos Alberto;MCDAID, Paul Oliver;O'NEILL, Padraig Mary;WONG, John Wing WO2012/25861, 2012, A1 Location in patent:Page/Page column 20

FullText