HRID1051514
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of 3-bromobenzene-1,2-diamine (2 g, 10.7 mmol) in HCOOH was stirred at 100° C. for 1 h. The mixture was cooled and concentrated in vacuo and diluted with ethyl acetate and aq. NaHCO3. The mixture was extracted further with ethyl acetate and the combined organic layers dried and concentrated to give the crude product which was purified by column chromatography to obtain the desired product (1.65 g, Yield 80%). LCMS (m/z): 197.0 (M+1).
WORKUP
后处理
- temperatureThe mixture was cooled
- concentrationconcentrated in vacuo
- additiondiluted with ethyl acetate and aq. NaHCO3
- extractionThe mixture was extracted further with ethyl acetate
- customthe combined organic layers dried
- concentrationconcentrated
- customto give the crude product which
- customwas purified by column chromatography