Triethylamine → 1,2-Dihydro-3-methyl-1-[4-(propan-1-ylsulfonamido)butan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one

To a solution of 1.22 g (5.0 mmol) of 1-[4-(amino) butan-1-yl]-1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one and 1.1 ml (7.9 mmol) of triethylamine in 40 ml of methylene chloride was added, while stirring under ice-cooling, 0.73 ml (6.5 mmol) of propan-1-ylsulfonyl chloride. The mixture was stirred for 0.5 hour at room temperature. The reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate, which was then dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was recrystallized from methylene chloride—methanol—ether to give 1.313 g of the desired compound (75.0%, pale brown crystals), m.p.150.0-151.0° C.

1. temperaturecooling
2. stirringThe mixture was stirred for 0.5 hour at room temperature
3. washThe reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate, which
4. dry with materialwas then dried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled off
6. customthe residue was recrystallized from methylene chloride—methanol—ether

ORD record

ord-ed6a3c4e40c14ed886fd5be68b049240

Source dataset

uspto-grants-2001_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06251905B1