Dimethylformamide → HCID 22641001, compound

Participants

Reaction Conditions

Reaction Steps

Thiocarbonyldiimidazole (4.56 g, 25.6 mmol) (Aldrich) was dissolved in N,N-dimethylformamide (25 mL) and the solution cooled to −15° C. A solution diethyl-[2-(4-nitro-phenoxy)-ethyl]-amine (5 g, 25.7 mmol) (from Step B above) in N,N-dimethylformamide (75 mL) was added dropwise and the mixture was then stirred at room temperature for 1 hour. The solution was cooled to 0° C. and poured into ice/water (1000 mL), stirred 30 minutes, and the precipitate was filtered off, washed with water and dried under high vacuum to give 4.95 g, (83%) diethyl-[2-(4-isocyanato-phenoxy)-ethyl]-amine. Mass spectrum (ES) MH+=251.

Provenance & Evidence