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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 20840Erstellt: 24. Oktober 2026

1,2-Dichloroethane → HCID 59347881, Verbindung

https://huagongshe.com/de/reaction/20840

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
Edukt1,2-DichloroethaneHCID 11—
Edukt1-HydroxybenzotriazoleHCID 75771—
EduktSodium BicarbonateHCID 516892—
Edukt2-Chloro-3-(trifluoromethyl)benzoic acidHCID 2736677—
Edukt[2-Methyl-2-(2-methyl-1-pyrrolidinyl)-1-phenylpropyl]amineHCID 59347786—
LösungsmittelDichloromethaneHCID 6344—
ProduktHCID 59347881HCID 59347881—

Reaktionsschritte

A mixture of [2-methyl-2-(2-methyl-1-pyrrolidinyl)-1-phenylpropyl]amine D26 (0.150 g; 0.647 mmol), 2-chloro-3-(trifluoromethyl)benzoic acid (0.174 g; 0.775 mmol), EDC (0.149 g; 0.777 mmol) and HOBt (0.020 g; 0.148 mmol) in DCM (4 ml) was shaken at room temperature for 66 hours. Saturated sodium hydrogen carbonate (8 ml) was added and shaking continued for 0.5 hours. The organic layer was passed through a phase separation cartridge and applied to a 2 g SCX column. The column was washed with DCM and methanol and the product eluted with 1M ammonia in methanol. The crude product was purified by chromatography on silica gel (20 g) eluting with 0-100% ethyl acetate in pentane gradient to afford the title compound as two pairs of enantiomers.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS07745642B2
Quelldatensatzuspto-grants-2010_06
ORD IDord-d442d140b910474784016bfda8a268a9
Quellennotizuspto-grants-2010_06