Cyclohexaneacetaldehyde, alpha-methyl- → HCID 18931636, compound

Participants

Reaction Steps

In a 2 L flask with a distillation tube attached thereto, 475 g of ethyl cyanoacetate (VI-1) (4.20 moles, 1.05 times by mole with respect to the 2-cyclohexylpropanal (II)), 6.0 g of acetic acid (0.10 millimole, 0.025 times by mole with respect to the 2-cyclohexylpropanal (II)), and 3.4 g of piperidine (40 millimoles, 0.01 times by mole with respect to the 2-cyclohexylpropanal (II)) were placed, which then was stirred at room temperature. Then, 561 g (4.00 moles) of 2-cyclohexylpropanal (II) (“Pollenal II” (Trade Name), manufactured by Kao Corporation) was dropped thereinto over 40 minutes. Thereafter, this was heated to 50° C., the pressure was reduced gradually to 4.0 kPa over two hours, and the reaction was continued while by-product water was removed. Furthermore, excessive ethyl cyanoacetate was distilled under 130 Pa at 110° C. Then, 921 g of the concentrated liquid thus obtained was subjected to gas chromatography quantitative analysis. As a result, the conversion ratio of the 2-cyclohexylpropanal (II) was 100% and the ethyl 2-cyano-4-cyclohexylpenta-2-enoate (VII-1) had a purity of 98.0% and a reaction yield of 95.9%.

Provenance & Evidence