o-Chlorobenzylidene malononitrile synthesis
- Product Name:o-Chlorobenzylidene malononitrile
- CAS Number:2698-41-1
- Molecular formula:C10H5ClN2
- Molecular Weight:188.61
Yield:2698-41-1 99.5%
Reaction Conditions:
Stage #1: malononitrile;piperidine in water at 20 - 30;
Stage #2: 2-chloro-benzaldehyde in water at 50;Product distribution / selectivity;Knoevenagel Condensation;
Steps:
1; II; III preparation of 2-chlorobenzylidenemalononitrile
Example 1 Water (5000 ml) was taken in a three-necked round bottom flask equipped with thermometer, pressure equalizing funnel and magnetic stirrer. To this malononitrile (660.6 g, 10 moles) was added and then piperidine (10mi, 0.1 mole) was added with constant stirring. To this 2-chlorobenzaldehyde (2108 g, 15 moles) was added slowly with continuous stirring through pressure equalizing funnel. The temperature of the reaction mixture was maintained at 50 C during addition of 2-chlorobenzaldehyde.The white crystalline solid CS thus obtained was filtered and then dried under vacuum (25mm). Mother liquor obtained after filtration of white solid was recycled for the preparation of CS by the same procedure as mentioned above for ten times. The mother liquor obtained after 10 cycles was taken in three-necked round bottom flask, to this sodium hydroxide 250g was added and the mixture was refluxed for 4 hrs. After cooling the mixture to 25 C and after analysis, the effluent was disposed off in the municipal drainage system. The yield and 'purity of CS was >99.5% and the melting point is 92-94 C (Reported mp 94 C).
References:
WO2005/108350,2005,A1 Location in patent:Example 1; II; III
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