Ethylamine → Thiophenecarboxamide,N-ethyl-

Temperature

0 °C

Neat thiophene-2-carbonyl chloride (1.46 g, 10 mmol) is added dropwise to a solution of ethylamine (70% wt/water) in Dichloromethane (8 mL) and Et3N at 0° C. Additional ethylamine (2.5 ml, 70% wt/water) is added to the reaction mixture and the reaction is stirred at 0° C. for 2 hrs and the warmed to room temperature for 2 h. The reaction mixture is transferred to a separatory funnel and the organic layer is washed sequentially with aqueous 1N HCl solution, water and saturated aqueous NaHCO3 solution. The organic phase is collected, dried over Na2SO4, filtered and concentrated to give the title compound (1.4 g, 90%).

1. temperaturethe warmed to room temperature for 2 h
2. customThe reaction mixture is transferred to a separatory funnel
3. washthe organic layer is washed sequentially with aqueous 1N HCl solution, water and saturated aqueous NaHCO3 solution
4. customThe organic phase is collected
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated

ORD record

ord-117c5ed339844ac9b40f822ad29d4e9f

Source dataset

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07977351B2