HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 61747Erstellt: 23. Oktober 2026
Ethanethiol, 2-(diethylamino)-, hydrochloride (1:1) → HCID 66833974, Verbindung
https://huagongshe.com/de/reaction/61747
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethanethiol, 2-(diethylamino)-, hydrochloride (1:1) | HCID 16031 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| Edukt | Trifluoro-methanesulfonic acid 3-cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yl ester | HCID 86663817 | — |
| Katalysator | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | 1,2-Dimethoxyethane | HCID 8071 | — |
| Produkt | HCID 66833974 | HCID 66833974 | — |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09440922B2 |
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| Quelldatensatz | uspto-grants-2016_09 |
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| ORD ID | ord-afc8fa3be38c4cf1bd6d0d54a4e6a27b |
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| Quellennotiz | uspto-grants-2016_09 |
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