Sodium Iodide → 3-Chloro-5-iodo-1-(4-isopropoxyphenyl)indole-2-carboxylic acid ethyl ester

温度

120 °C

A mixture of 5-bromo-3-chloro-1-(4-isopropoxyphenyl)-1H-indole-2-carboxylic acid ethyl ester (2.80 g, 6.44 mmol) (prepared in accordance with the procedure described in Example 35, Method 1, step (b)), CuI (122 mg, 0.64 mmol), NaI (1.94 g, 12.9 mmol), N,N′-dimethyl-1,2-diaminoethane (142 μL, 1.28 mmol) and 1,4-dioxane (10 ml) was stirred at 120° C. for 24 h. The mixture was cooled to room temperature and diluted with EtOAc (200 ml). The combined organic phase was washed with diluted NH4OH solution (2×200 mL), HCl (0.1 N solution; 2×200 mL), brine (100 mL) and dried over Na2SO4. Filtration and concentration of the organic phase gave the sub-title compound (3.02 g 97%).

1. customprepared in accordance with the procedure
2. temperatureThe mixture was cooled to room temperature
3. washThe combined organic phase was washed with diluted NH4OH solution (2×200 mL), HCl (0.1 N solution; 2×200 mL), brine (100 mL)
4. dry with materialdried over Na2SO4
5. filtrationFiltration and concentration of the organic phase

ORDレコード

ord-6b482356963042a8bfe69931bdc07ee5

出典データセット

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07705023B2