Triethylamine → HCID 45739920, Verbindung

Boc-D-Pro-OH (209 mg, 0.970 mmol) was dissolved in DMF (4 mL), followed by addition of the HBTU (552 mg, 1.46 mmol) and Triethylamine (270 μL). The solution was stirred at room temperature for 30 minutes prior to the addition of piperonylamine (121 μL, 0.970 mmol). The reaction mixture stirred at rt for 16 h then the solution was transferred to a separatory funnel containing DCM (50 mL). The organic layer was washed with NaHCO3 (2×50 mL, sat. aq.) and dried over Na2SO4. The solution was concentrated and purified by prep LCMS to afford 278.0 mg (82.5%) of 2-[(benzo[1,3]dioxol-5-ylmethyl)-carbamoyl]-pyrrolidine-1-carboxylic acid tert-butyl ester. [M+H]+ 349.09.

1. stirringThe reaction mixture stirred at rt for 16 h
2. customthe solution was transferred to a separatory funnel
3. washThe organic layer was washed with NaHCO3 (2×50 mL, sat. aq.)
4. dry with materialdried over Na2SO4
5. concentrationThe solution was concentrated
6. custompurified by prep LCMS

ORD-Eintrag

ord-b344dd2db00e4e54bb5f2f341e6142cd

Quelldatensatz

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07825256B2