Bromine → HCID 13084274, compound

Participants

Reaction Steps

To a suspension of 2-thioxo-benz[cd]indole-1(2H)-acetic acid (4.2 g, 17.26 mmol, described in Example 6), in glacial acetic acid (80 mL) was added a solution of bromine (3.59 g, 22.44 mmol) in glacial acetic acid (20 mL) in two portions with mechanical stirring within one hour. After initial clearing of the suspension, a heavy precipitate was formed. More acetic acid (60 mL) was added in order to make stirring more efficient. The mixture was filtered and the precipitate was washed twice with water (150 mL), dried, crystallized from ethanol-water giving 4.7 g in two crops and recrystallized from methanol to give 3.0 g of the title compound, identical in all respects to that prepared in Example 6.

Provenance & Evidence