Trichloroacetic Acid → HCID 18323957, compound

Participants

Reaction Conditions

Reaction Steps

Trichloracetic acid (31.9 g, 195 mmoles) is dissolved in chloroform (200 ml). Sodium azide (8.45 g, 130 mmoles) is added and the medium is cooled down to 10° C. The alcohol obtained in Stage 17a (11.8 g, 65 mmoles) dissolved in chloroform (50 ml) is added dropwise. The reaction medium is agitated for 48 hours whilst maintaining the temperature at 10-12° C. A solution of ammonium hydroxide (10%) is then added until neutralisation, then the aqueous phase is extracted with dichloromethane (3×100 ml). The organic phase is washed with water (200 ml), dried over Na2SO4 and concentrated to dryness. In this way, a brown oil is obtained which is then used without further purification.

Provenance & Evidence