反应详情

To the derivative 2,4-dibromobutyryl bromide (3.1 g) in dry dichloromethane (60 ml) pyridine (3.2 ml was added, the mixture was kept at 0° C. under a nitrogen atmosphere for 10 minutes and then the N-t-butoxy carbonyl-1,4 phenylene diamine (2.08 g) was dropped. After 1 hour the mixture was poured into a saturated solution of NH4Cl (200 ml) extracted with EA (3×150 ml) and the organic phase washed with brine (200 ml), dried and concentrated in vacuum, the crude was purified by flash chromatography (eluting with CH/EA 80:20) to give of the title compound as a yellow foam (3.5 g ). T.I.c. CH/EA 8:2, Rf=0.53.

1. extractionextracted with EA (3×150 ml)
2. washthe organic phase washed with brine (200 ml)
3. customdried
4. concentrationconcentrated in vacuum
5. customthe crude was purified by flash chromatography (eluting with CH/EA 80:20)