Sulfamic Acid → HCID 961607, compound

Participants

Reaction Conditions

Reaction Steps

Sulfamic acid (17.28 g, 178 mmol) was added to a solution of 9 (21.11 g, 80.5 mmol) in acetone (420 ml) and water (210 ml) at 0° C. Over a period of 20 minutes, 80% NaClO2 (10.42 g, 92.2 mmol) was added at 0° C. The solution was stirred at 0° C. for 30 minutes and then concentrated to about 200 ml. After dilution with water (200 ml), the mixture was extracted with CH2Cl2 (1×200 ml, 2×100 ml). The organic layer was dried (MgSO4) and concentrated. Crystallization from cyclohexane/ethyl acetate (1:1) generated 19.12 g (85%) of 10 as pale yellow crystals, mp 127°-128° C. (lit. mp 128°-130° C.).

Provenance & Evidence