Dichloroacetic Acid → HCID 20067568, compound

Participants

Reaction Steps

Sodium acetate (5.7 g) and dichloroacetic acid (8.5 ml) were stirred together in dichloromethane (8.5 ml) at 0° C. for 5 minutes then hydroxylamine hydrochloride (4.8 g) added. After 1 h at room temperature more dichloromethane (17 ml) was added and after a further 30 minutes, the product from Example 7. Step A (1.9q) was added. After 1 h at room temperature the reaction mixture was poured into ice-water (200 ml) and washed with ammonia solution (70 ml). The organic layer was dried (Na2SO4), filtered and concentrated in vacuo to give the required product (2.04 g) as a colourless form. Spectral data were consistent with the proposed structure.

Provenance & Evidence