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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 77401Erstellt: 25. Oktober 2026

Lithium Hydroxide → HCID 69928688, Verbindung

https://huagongshe.com/reaction/77401

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktLithium HydroxideHCID 3939—
EduktEthyl orthoformateHCID 31214—
Edukt2-amino-N-methyl-5-(5-methylhexahydropyrrolo[3,4-c]pyrrole-2(1H)-yl)benzamideHCID 69928598—
LösungsmittelMethanolHCID 887—
ProduktHCID 69928688HCID 69928688—

Reaktionsbedingungen

Temperatur160 °C

Reaktionsschritte

2-Amino-N-methyl-5-(5-methylhexahydropyrrolo[3,4-c]pyrrole-2(1H)-yl)benzamide (Intermediate 8A) (100 mg, 0.36 mmol) was dissolved in triethoxymethane (1 mL) and sealed in a microwave vial. Heated at 160° C. for 10 minutes. Reaction allowed to cool to room temperature and lithium hydroxide solution added (0.5 mL, 1M in methanol) and reaction stirred overnight. Organic layer loaded onto a 1 g SCX cartridge. The crude material was purified by SCX, and the solvent removed under reduced pressure. The crude material was then re-dissolved in methanol (1 mL) and purified by preparative-HPLC. Purified sample was free-based using 500 mg SCX cartridge to afford 3-methyl-6-(5-methylhexahydropyrrolo[3,4-c]pyrrole-2(1H)-yl)quinazolin-4(3H)-one (56 mg, 0.2 mmol).

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08841289B2
Quelldatensatzuspto-grants-2014_09
ORD IDord-7d2bf6bfb9384f03b91ce19946d24598
Quellennotizuspto-grants-2014_09