1,4-Dioxane → HCID 15027354, compound

Participants

Reaction Conditions

Reaction Steps

The crude hydroxylamine (4.2 g, 0.02 mol) from Example 1 is dissolved in dioxane (80 ml) and water (50 ml). The turbid solution is cooled to -5° C. and then treated with NaOAc (3.3 g, 0.04 mol) followed by ethyl oxalylchloride (3.0 g, 0.022 mol). The mixture is stirred at 24° C. for 3.0 hours, poured onto ice-1N HCl (40 mL) and extracted with CH2Cl2. The extract is washed with brine, water and dried over Na2SO4. The solvent is distilled off to give (9H-fluoren-2-ylmethyl)hydroxyamino-oxo-acetic acid, ethyl ester which is fractionally recrystallized from isopropyl ether and CH2Cl2 and then from isopropyl ether. Yield 1.6 g (26%); mp 130°-131° C.

Provenance & Evidence