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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 713889Erstellt: 25. Oktober 2026

Dichloromethane → HCID 178451617, Verbindung

https://huagongshe.com/reaction/713889

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktDichloromethaneHCID 6344—
EduktCesium carbonateHCID 10796—
EduktN-Boc-5-HydroxyindolineHCID 10657398—
EduktMethanesulfonic acid 4-tert-butyl-cyclohexyl esterHCID 11128255—
Lösungsmitteltert-ButanolHCID 6386—
LösungsmittelMethyl Ethyl KetoneHCID 6569—
ProduktHCID 178451617HCID 178451617100%

Reaktionsbedingungen

Temperatur100 °C

Reaktionsschritte

A mixture of 5-hydroxy-2,3-dihydro-indole-1-carboxylic acid tert-butyl ester (0.6 g, 2.6 mmol) in tert-butyl alcohol (8 ml) and 2-butanone (4 mL) was added cesium carbonate (2.5 g, 7.7 mmol) followed by methanesulfonic acid 4-tert-butyl-cyclohexyl ester (1.9 g, 7.7 mmol). The mixture was heated in a sealed vial at 100° C. over night to form precipitate. The mixture was treated with dichloromethane and the precipitate was filtered off and the solvent was concentrated. The residue was purified with a silica gel column eluted with ethyl acetate in hexanes from 0 to 30% to give precipitate (0.96 g, yield: 100%). ESI-MS: 373.30 (M)+.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS09186367B2
Quelldatensatzuspto-grants-2015_11
ORD IDord-2c210c25e06a49b29d6831d82278e2e9
Quellennotizuspto-grants-2015_11