1,1'-Carbonyldiimidazole → HCID 18976547, compound

Participants

Reaction Steps

82.7 g (0.51 mol) of 1,1'-carbonyldiimidazole in 5.0 l of tetrahydrofuran are allowed to react as described in Example 1, with 93.08 g (0.5 mol) of 3-(3,5,5-trimethyl-2,4-dioxoimidazolidin-1-yl)propionic acid and are subsequently reacted with 53.62 g (0.51 mol) of 2-aminoacetaldehyde dimethyl acetal. The reaction mixture is evaporated in a rotary evaporator, and the imidazole present in the residue is removed by distillation at a bath temperature of 120° C./0.1 mmHg for 3 hours, giving 134.1 g (98.1% of theory) of a brownish, liquid crude product, which is recrystallized from 130 ml of ethyl acetate, giving 88.1 g (65.0% of theory) of colourless, crystalline N-(2,2-di methoxyethyl)-3-(3,5,5-trimethyl-2,4-dioxoimidazolidin-1-yl)propionamide, whose melting point is 86.4° C.

Provenance & Evidence