HCID 54212570, compound → HCID 23289830, compound

Participants

Reaction Conditions

Reaction Steps

Under nitrogen, titanium tetrachloride (1.2 ml; 2.1 g; 11.0 mmol) was added to the above enamine (Example 38) (2.2 g, 10.0 mmol) and the stirred mixture was heated at 140° C. for 1 hour. After cooling, sodium hydroxide (10M, 20 ml) was added and the mixture heated under reflux for 1 hour. After being allowed to cool, this was filtered and the solids were washed with dichloromethane. Any organics in the filtrate were also extracted into dichloromethane, the extracts were combined, dried (Na2SO4), filtered and the solvent evaporated. Kugelrohr distillation (180° C., 0.02 mmHg) gave the product as a very pale yellow powder.

Provenance & Evidence