2,4-dioxo-3-azaspiro[5.5]undecane-1,5-dicarbonitrile synthesis
- Product Name:2,4-dioxo-3-azaspiro[5.5]undecane-1,5-dicarbonitrile
- CAS Number:4355-15-1
- Molecular formula:C12H13N3O2
- Molecular Weight:231.25
108-94-1
594 suppliers
$12.00/50g
105-56-6
458 suppliers
$10.00/5ml
107-91-5
576 suppliers
$5.00/10g
4355-15-1
19 suppliers
$172.00/250mg
Yield:4355-15-1 88%
Reaction Conditions:
with triethylamine in methanol at 25 - 30; for 8 h;Product distribution / selectivity;
Steps:
1.1
1. Preparation of 1,5-dicyano-2,4-dioxo-3-azaspiro[5,5]-undecane 98 g (1 mol) of cyclohexanone, 113 g (1 mol) of ethyl cyanoacetate, 84 g (1 mol) of cyanoacetamide, and 100 ml of methanol were mixed in a reaction flask. 101 g (1 mol) of triethylamine was added dropwise under stirring, and the reaction mixture was stirred for 8 hours with the temperature controlled within the range of 25°C to 30°C, and then was cooled and filtered. The filter cake was suspended in water, and the suspension was adjusted to pH 2-3 with concentrated hydrochloric acid while stirring. The suspension was filtered, washed with water, and dried to provide 1,5-dicyano-2,4-dioxo-3-azaspiro[5,5]-undecane. Yield: 88%, melting point: 202 to 210°C.
References:
EP1939170,2008,A1 Location in patent:Page/Page column 4-5
108-94-1
594 suppliers
$12.00/50g
105-56-6
458 suppliers
$10.00/5ml
4355-15-1
19 suppliers
$172.00/250mg
6802-76-2
32 suppliers
$100.00/100mg
105-56-6
458 suppliers
$10.00/5ml
4355-15-1
19 suppliers
$172.00/250mg