Borane;tetrahydrofuran → octahydro-2H-pyrazino[1,2-a]pyrazine

Temperatur

50 °C

To a suspension of hexahydro-2H-pyrazino[1,2-a]pyrazin-1(6H)-one (D78, 339 mg, 2.184 mmol) in 3.5 mL of THF kept at 0° C. were added dropwise 21.84 mL of a 1M borane-THF solution. The reaction was kept at 75° C. under nitrogen atmosphere for 3 h, then quenched by slow addition MeOH at 0° C. After 30 min at room temperature, 5 mL of a 37% HCl aqueous solution diluted in 10 mL of MeOH were added and the resulting solution was heated to 50° C. for 2.5 h. The solvent was removed and the residue purified by SCX, leaving 251 mg of the title compound.

1. customkept at 0° C.
2. customquenched by slow addition MeOH at 0° C
3. waitAfter 30 min at room temperature
4. addition5 mL of a 37% HCl aqueous solution diluted in 10 mL of MeOH
5. additionwere added
6. customThe solvent was removed
7. customthe residue purified by SCX

ORD-Eintrag

ord-41fc832699884a1a8ffb99dfbef9bb08

Quelldatensatz

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08097618B2