Methylamine → HCID 22164323, compound

Participants

Reaction Steps

21 g of a 30% strength aqueous methylamine solution were added dropwise at approx. -75° C. in the course of 45 minute$ to 25.25 g (0.1 mol) Df 2,4-dichloro-thiazole-sulphonyl chloride from Example 1 in 250 ml of the cold bath was then removed and the temperature was subsequently allowed to rise to room temperature, the mixture was subsequently stirred for 30 minutes, the resulting suspension was evaporated under a waterpump vacuum, and the residue was stirred with 300 ml of water. The solid was filtered off with suction and chromatographed on silica gel (eluent toluene/EtOH 15:1) in order to remove small amounts of starting material and product which is substituted in the 2-position. 22 g of product were obtained (89% of the theoretical yield) m.p.: 72-3° C.

Provenance & Evidence