反应 #1269898
ord-b1fdffb1790a4a76999b951b6d7b47b4
反应方程式
N-Bromosuccinimide
8-chloro-4H,6H-2,3,5,10b-tetraaza-benzo[e]azulene-5-carboxylic acid tert-butyl ester
→
1-bromo-8-chloro-4H,6H-2,3,5,10b-tetraaza-benzo[e]azulene-5-carboxylic acid tert-butyl ester
收率 85.0%
反应物
试剂
无
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他for 2 hours
- 2其他The solvent was removed in vacuo
- 3其他the residue was purified by chromatography (50 g silica gel, heptane: ethylacetate 1:9 to 1:0)
实验过程
N-Bromosuccinimide (4.50 g, 24.0 mmol) was added to 8-chloro-4H,6H-2,3,5,10b-tetraaza-benzo[e]azulene-5-carboxylic acid tert-butyl ester (7.00 g, 21.8 mmol) in tetrahydrofuran (140 ml). The mixture was stirred in boiling tetrahydrofuran for 2 hours. The solvent was removed in vacuo and the residue was purified by chromatography (50 g silica gel, heptane: ethylacetate 1:9 to 1:0) to yield 7.39 g (85%) 1-bromo-8-chloro-4H,6H-2,3,5,10b-tetraaza-benzo[e]azulene-5-carboxylic acid tert-butyl ester as white solid. MS m/e: 401 (M+H+).