Ammonia → HCID 21318015, compound

Participants

Reaction Steps

To a suspension of 3.5 g (0.014 mole) of 5-(1-cyclohexen-1-ylthio)-2-nitrobenzene-amine in 125 ml of absolute ethanol under N2 there is added a solution of 8.4 g of Na2S2O4, 8.4 ml of concentrated aqueous ammonia and 52.5 ml of water. The mixture is refluxed for 15 minutes and an additional 0.8 g of Na2S2O4 is added. After an additional 15 minutes reflux period TLC (silica, Et2O) shows no starting material present. The ethanol is removed in vacuo; the aqueous residue is taken to pH 12 with 50% aqueous NaOH and then extracted with CH2Cl2. The organic extracts are combined, dried (MgSO4) and evaporated to give an oil which is used immediately in the following reaction.

Provenance & Evidence