1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 86650785, compound

Participants

Reaction Steps

The compound (2.32 g, 6.13 mmol) obtained in step A, the compound of Reference Example 3 (1.67 g, 8.26 mmol) and 1-hydroxybenzotriazole (1.19 g, 8.81 mmol) were dissolved in an N,N-dimethylformamide (3 ml)-dichloromethane (40 ml) mixed solvent, WSC (1.80 g, 9.39 mmol) was added under ice-cooling, and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with an ethyl acetate-hexane=1:1 (250 ml) mixed solvent, washed with water, 10% aqueous citric acid solution, diluted aqueous sodium hydroxide solution and saturated brine, and dried over anhydrous magnesium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure. The obtained solid was washed with a diethyl ether-hexane=1:1 mixed solvent, and dried under reduced pressure to give the title compound (2.81 g, yield 81%) as a colorless solid.

Provenance & Evidence