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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 448825Erstellt: 26. Oktober 2026

Triethylamine → HCID 24855800, Verbindung

https://huagongshe.com/reaction/448825

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktTriethylamineHCID 8471—
EduktDiethyl cyanophosphonateHCID 76257—
EduktN2,N2-dimethylpyridine-2,5-diamineHCID 78642—
Edukt5-fluoro-1-(3-fluorobenzyl)-1H-indole-2-carboxylic acidHCID 57431513—
LösungsmittelDimethylformamideHCID 6228—
ProduktHCID 24855800HCID 24855800—

Reaktionsschritte

0.27 ml (1.67 mmol) of diethyl cyanophosphonate is added dropwise at 20° C. under argon to a solution of 0.4 g (1.39 mmol) of 5-fluoro-1-(3-fluorobenzyl)-1H-indole-2-carboxylic acid (obtained in Example 1.1) and 0.229 g (1.67 mmol) of 3-amino-6-(dimethylamino)pyridine in 3.5 ml of dry dimethylformamide. The mixture is stirred for 10 minutes and then 0.43 ml (3.06 mmol) of triethylamine is added dropwise. The mixture is stirred at ambient temperature for 18 hours and concentrated under reduced pressure, and then the residue is taken up in 50 ml of ethyl acetate. This solution is then successively washed with three times 20 ml of a saturated sodium hydrogencarbonate solution, 50 ml of water and 20 ml of a saturated sodium chloride solution and then dried over sodium sulfate, filtered and concentrated under reduced pressure. The solid obtained is triturated from hot isopropyl ether. 0.423 g of a solid is collected by filtration, which solid is dried under reduced pressure and used as in the following stage.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08481745B2
Quelldatensatzuspto-grants-2013_07
ORD IDord-67b8ef6dddf342d9aa08ef3e16317729
Quellennotizuspto-grants-2013_07