Ethyl potassium malonate synthesis
- Product Name:Ethyl potassium malonate
- CAS Number:6148-64-7
- Molecular formula:C5H7KO4
- Molecular Weight:170.2
105-53-3
6148-64-7
Step 1: Add diethyl malonate (100g, 0.625mol) and anhydrous ethanol (400ml) to a 2 liter round bottom flask fitted with a magnetic stirrer. A solution of potassium hydroxide (35 g, 0.624 mol) in anhydrous ethanol (400 ml) was slowly added dropwise at room temperature. After the dropwise addition, the reaction mixture was continued to be stirred overnight. Subsequently, the reaction mixture was heated to reflux and then slowly cooled to room temperature. The first products were isolated by vacuum filtration through a large No. 2 sintered glass funnel and dried at room temperature for 1 hour. The filtrate was concentrated to about 500 ml and then cooled to room temperature to precipitate the second batch of crystals. Combining the two batches of product, the total yield was 97.7 g with 92% yield.
105-53-3
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6148-64-7
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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 2nd 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
1071-46-1
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6148-64-7
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