Triethylamine → 5-Bromo-3-[(1,1-dioxidotetrahydro-3-thienyl)methyl]-1H-indole-7-carboxamide

온도

20 °C

TBTU (5.68 g, 17.68 mmol) and triethylamine (1.79 g, 17.68 mmol) were added to a solution of 5-bromo-3-[(1,1-dioxidotetrahydro-3-thienyl)methyl]-1H-indole-7-carboxylic acid (3.28 g, 8.84 mmol) in dichloromethane (100 mL). After the mixture was stirred for 0.5 h at 20° C., NH3/MeOH was added into the solution, and stirring continued for 2 h. The mixture was washed with water and extracted with EtOAc. The organic phase was dried (Na2SO4) and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel (petroleum: ethyl acetate=10:1 to 5:1 to 2:1), giving 1.1 g (33.6%) of the title compound.

1. stirringstirring
2. waitcontinued for 2 h
3. washThe mixture was washed with water
4. extractionextracted with EtOAc
5. dry with materialThe organic phase was dried (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified by column chromatography on silica gel (petroleum: ethyl acetate=10:1 to 5:1 to 2:1)

ORD 기록

ord-493861ac05414ce2abaf03139f036af2

출처 데이터셋

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08372875B2