Ammonium Chloride → HCID 10805252, compound

Participants

Reaction Steps

To a solution of N-[5-(4-chlorophenylthio)thien-2-ylmethyl]hydroxylamine (6.65 g) in dioxan (100 ml) at room temperature under nitrogen, was added trimethylsilylisocyanate (4.25 g) and the resulting solution stirred for 2 hours, poured onto saturated aqueous ammonium chloride, extracted with ether (2×100 ml), dried over MgSO4 and evaporated under reduced pressure to give a yellow oil. The oil was flash chromatographed on a Sorbsil C60-40/60H column using ether to give a white solid. Recrystallised from ether/petroleum ether (40°-60° C.) to give a white crystalline solid m.p. 158°-160° C.

Provenance & Evidence