Carbon tetrabromide → HCID 69067664, compound

Participants

Reaction Steps

To a solution of 0.400 g (4R,9aR)-7-bromo-6-hydroxymethyl-4-methyl-3,4,9,9a-tetrahydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester (example 21 step 1) in 5 ml dichloromethane was added at room temperature 0.4 g triphenylphosphine and carbontetrabromide and the mixture was stirred at room temperature for 30 min. The red-orange solution was purified by chromatography on silica gel with heptane:ethyl acetate=1:1. The product fractions were collected and evaporated. The resulting oil (showing crystal seeds) was triturated with hexane. The crystalline solid was collected and dried to constant weight to yield 0.307 g of the title compound (MS: 406.1; 404.2 (M+H+)).

Provenance & Evidence