反应详情

温度

-15 °C

Thiocarbonyldiimidazole (438 mg, 2.46 mmol) (Aldrich) was dissolved in dimethylformamide (10 mL) and the solution was cooled to −15° C. A solution [2-(4-amino-phenoxy)-ethyl]-ethyl-carbamic acid tert-butyl ester (750 mg, 2.35 mmol) (from step C above) in dimethylformamide (25 mL) was added dropwise, stirred at room temperature for 90 minutes and poured into ice/water. After stirring 30 minutes the precipitate was filtered off, washed with water, and dried under high vacuum to give 453 mg (53%) of ethyl-[2-(4-isothiocyanato-phenoxy)-ethyl]-carbamic acid tert-butyl ester. Mass spectrum (ES) MH+=323.

1. stirringAfter stirring 30 minutes the precipitate
2. filtrationwas filtered off
3. washwashed with water
4. customdried under high vacuum