Hydrochloric Acid → HCID 14013848, compound

Participants

Reaction Steps

To a mechanically stirred mixture of 11.52 g of (0.087 mol) of copper (II) chloride, and 11.18 g (0.108 mol) of t-butylnitrite in 350 ml of CH3CN, was added a solution of 25.00 g (0.070 mol) of product of Example 100 in 25 ml of CH3CN in such a rate that a slow evolution of N2 was observed. After 18 hours the mixture was poured into 3.7% HCl, and extracted with diethyl ether. The ether phase was washed with H2O, and dried (MgSO4). This was concentrated in vacuo to 24.03 g of a yellow oil. The crude product was purified by HPLC in 5% ethyl acetate/cyclohexane affording 13.2 g (50%) of product as a yellow solid; mp 35°-40° C.

Provenance & Evidence