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HRID 61747Erstellt: 23. Oktober 2026

Ethanethiol, 2-(diethylamino)-, hydrochloride (1:1) → HCID 66833974, Verbindung

https://huagongshe.com/de/reaction/61747

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktEthanethiol, 2-(diethylamino)-, hydrochloride (1:1)HCID 16031—
EduktDiisopropylethylamineHCID 81531—
Edukt1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 636044—
EduktTrifluoro-methanesulfonic acid 3-cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yl esterHCID 86663817—
KatalysatorBis(dibenzylideneacetone)palladiumHCID 9811564—
LösungsmittelWaterHCID 962—
Lösungsmittel1,2-DimethoxyethaneHCID 8071—
ProduktHCID 66833974HCID 66833974—

Reaktionsbedingungen

Temperatur160 °C

Reaktionsschritte

Trifluoro-methanesulfonic acid 3-cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yl ester (Compound B1, 25 mg, 0.057 mmol) was dissolved in dimethoxyethane (0.5 mL), added with 2-diethylaminoethanethiol hydrochloric acid salt (19.6 mg, 2 eq.), Pd2(dba)3 (2.6 mg, 0.05 eq.), Xantphos (3.3 mg, 0.1 eq.) and DIPEA (0.06 mg, 6 eq.), and the mixture was stirred at 160° C. for 30 min. The reaction solution was added to water, extracted with ethyl acetate, and dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (dichloromethane/methanol) to obtain the target compound (white amorphous, 22.4 mg, 93%).

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS09440922B2
Quelldatensatzuspto-grants-2016_09
ORD IDord-afc8fa3be38c4cf1bd6d0d54a4e6a27b
Quellennotizuspto-grants-2016_09