Chloroform → HCID 178463596, compound

Participants

Reaction Conditions

Reaction Steps

The product of step (i) (11.85 g) was dissolved in 2N NaOH (270 ml) and 10N NaOH (27 ml) and heated to 65° C. Within 1.25 hours 50% Ni-Al alloy (518 mmoles. of Ni and 1125 mmols of Al) (60.8 g) was added under vigorous stirring at 65-70° C. After a further 0.75 hr at the same temperature the reaction mixture was cooled to room temperature and treated with chloroform (400 ml). The nickel was filtered off and washed with 350 ml of chloroform and 150 ml of water. The filtrate was separated and the chloroform layer evaporated to dryness. The residue (19.64 g) was dissolved in acetone (100 ml), treated with 2 portions of charcoal (0.15 g) filtered and evaporated. The residue was treated with diethylether (100 ml) and crystals collected (6.10 g), mp 80-9° C. A second , crop gave 1.25 g. A recrystallized sample from diisopropylether had mp 103-105° C.

Provenance & Evidence