Dimethylformamide → HCID 57729052, compound

Participants

Reaction Steps

A suspension of N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (1.14 g, 5.93 mmol) and triethylamine (4 ml) in N,N-Dimethylformamide (30 ml) is stirred at room temperature. Then, 1-Hydroxybenzotriazole (0.698 g, 4.56 mmol), 7,8-Dimethoxy-1,2,2a,3,4,5-hexahydro-3-aza-acenaphthylene hydrochloride (1.0 g, 4.56 mmol) and N-acetil-3-aminopropanoic acid (0.657 g; 5.0 mmol) were added and the crude is stirred at room temperature for 15 h. Then, water (60 ml) and CH2Cl2 (60 ml) are added to the crude. Organic layer is separated and the aqueous one is extracted with CH2Cl2 (2×60 ml). All the organic layers were collected and washed with 0.1 N HCl (3×60 ml), with NaHCO3 (3×60 ml) sat and with water (3×40 ml). After drying with Na2SO4, filtration and vacuum concentration, a beige oil is obtained (1.32 g, 87% yield). The oil is cristallized in ethyl acete to give a beige solid (1.0 g, 66% yield).

Provenance & Evidence