3,3,3-Trifluoropropene → Methyl 3-((3,3,3-Trifluoropropyl)Thio)Propionate

Temperatur

20 °C

A 100 mL stainless steel Pan reactor was charged with methyl 3-mercaptopropionate (4.15 g, 34.5 mmol), toluene (30.3 g), and 2,2′-azobis(4-methoxy-2,4-dimethyl) valeronitrile (V-70, 0.531 g, 1.72 mmol) and the reactor was cooled with a dry ice/acetone bath, purged with nitrogen, and pressure checked. 3,3,3-Trifluoropropene (3.40 g, 35.4 mmol) was added via transfer cylinder and the reaction was allowed to warm to 20° C. After 23 hours the reaction was heated to 50° C. for 1 hour to decompose any remaining V-70 initiator. The reaction was allowed to cool to room temperature. The solution was concentrated to provide the title compound (7.01 g, 66%, 70.3 wt % linear isomer by GC internal standard assay, 4.93 g active, 66%, 24:1 linear:branched by GC, 18:1 linear:branched by fluorine NMR)

1. temperaturethe reactor was cooled with a dry ice/acetone bath
2. custompurged with nitrogen, and pressure
3. temperatureAfter 23 hours the reaction was heated to 50° C. for 1 hour
4. temperatureto cool to room temperature
5. concentrationThe solution was concentrated

ORD-Eintrag

ord-725da699a8204c3bbc0005a7d128dc0f

Quelldatensatz

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09434712B2