4-Methylmorpholine → HCID 15631179, compound

Participants

Reaction Steps

An aliquot (1.0 g) of the resulting ester was dissolved in 30 ml of methylene chloride, and 0.21 g of N-methylmorpholine and 1.07 g of N-(3,4-methylenedioxybenzyloxycarbonyloxy)succinimide were added, and the mixture was stirred at room temperature for 3 hours. The reaction mixture was washed successively with saturated aqueous sodium bicarbonate solution, 5% aqueous potassium hydrogensulfate solution, and water, dried over anhydrous sodium sulfate, and concentrated to dryness under reduced pressure. The residue was recrystallized from ethanol/methanol to give 1.1 g of ethyl 1-[N2 -(3,4-methylenedioxybenzyloxycarbonyl)-N6 -(3-nitro-2-pyridinesulfenyl)-L-lysyl-O1 -ethyl-gamma-D-glutamyl]indoline-2(S)-carboxylate. mp. 130°-135° C. [α]D27 : -23.2° (dimethylformamide).

Provenance & Evidence