HRID1777691
反应详情
EQUATION
反应方程式
REACTANTS
反应物
HCID81531
Diisopropylethylamine
C8H19N
HCID292331
4-(phenylamino)benzoic acid
C13H11NO2
HCID2827494
5-Chloro-1H-indole-3-ethylamine monohydrochloride
C10H12Cl2N2
HCID9886157
Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
C10H15F6N6OP
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 4-(phenylamino)benzoic acid (0.048 g, 0.225 mmol), 2-(5-chloro-1H-indol-3-yl)ethanamine hydrochloride (0.052 g; 0.225 mmol), HATU (0.094 g; 0.247 mmol) and N,N-diisopropylethylamine (0.097 mL; 0.563 mmol) in DMF (5 mL), was stirred at room temperature overnight. The reaction mixture was partitioned between ethyl acetate and sodium hydrogen sulphate, the organic layer was washed with sodium carbonate, brine, dried and concentrated in vacuo. The crude mixture was purified by flash chromatography on silica (eluent 20 to 100% ethyl acetate in heptane) to yield 0.024 g (27%) of the title compound as a yellow solid.
WORKUP
后处理
- customThe reaction mixture was partitioned between ethyl acetate and sodium hydrogen sulphate
- washthe organic layer was washed with sodium carbonate, brine
- customdried
- concentrationconcentrated in vacuo
- customThe crude mixture was purified by flash chromatography on silica (eluent 20 to 100% ethyl acetate in heptane)