Zurück
HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 218013Erstellt: 24. Oktober 2026

Trifluoroacetic acid → HCID 45279959, Verbindung

https://huagongshe.com/de/reaction/218013

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktTrifluoroacetic acidHCID 6422—
EduktDiisopropylethylamineHCID 81531—
EduktSodium BicarbonateHCID 516892—
EduktPyBOPHCID 2724699—
Edukt5-Cyanopyridine-2-carboxylic acidHCID 12400734—
Edukttert-butyl (+/-)-[(4aR*,8aS*)-8a-(6-amino-2,2-difluorobenzo[1,3]dioxol-4-yl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-2-yl]carbamateHCID 59281180—
LösungsmittelWaterHCID 962—
LösungsmittelDichloromethaneHCID 6344—
ProduktHCID 45279959HCID 45279959—

Reaktionsschritte

5-Cyanopyridine-2-carboxylic acid (4.0 mg), diisopropylethylamine (11.5 μl) and PyBOP (17.6 mg) were added to a solution of tert-butyl (±)-[(4aR*,8aS*)-8a-(6-amino-2,2-difluorobenzo[1,3]dioxol-4-yl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-2-yl]carbamate (10 mg) in dichloromethane (2.0 ml) in an ice bath. The mixture was heated to room temperature and stirred for four hours. The solvent was evaporated under reduced pressure and the residue was purified by NH-pTLC to obtain an intermediate. The resulting intermediate was dissolved in dichloromethane (3.0 ml) and TFA (1.0 ml) was added. After stirring at room temperature for four hours, the reaction solution was diluted with water and neutralized with a sodium bicarbonate solution. The aqueous layer was extracted with dichloromethane, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by NH-pTLC to obtain the title compound.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08198269B2
Quelldatensatzuspto-grants-2012_06
ORD IDord-39bc75924af84a62a8b718f43cc4731a
Quellennotizuspto-grants-2012_06