Triethylamine → HCID 21226931, compound

Participants

Reaction Conditions

Reaction Steps

A solution of thiophosgene (2.3 ml, 30 mmol) in THF (300 ml) was added dropwise to a solution containing N1-Methyl-4-nitro-benzene-1,2-diamine (5.01 g, 30 mmol) and Et3N (9.2 ml, 66 mmol) in THF (300 ml) at 0° C. over 90 min. After stirring at 0° C. for another 1 hr, the mixture was allowed to warm to room temperature. The mixture was then concentrated to about 100 ml, water (200 ml) was added, the mix was stirred for 20 min, the product was collected by filtration and washed with small amount of cold CH2Cl2, after drying left 5.16 g as a mustard yellow solid: LC/MS (m/e) at 210.0 [M+H]+, Rt at 1.49 min.

Provenance & Evidence