4-Bromo-1,1,2-trifluorobut-1-ene → 3,4,4-Trifluoro-3-butenyl dithiocarbamate

Temperatur

40 °C

2.8 g (25 mmol) of ammonium dithiocarbamate in 40 ml of ethanol are admixed dropwise with 5.32 g (26.3 mmol; purity 93.2%) of 4-bromo-1,1,2-trifluoro-1-butene, stirred at 40° C. for 3 h, another 2.8 g of ammonium dithiocarbamate is added after 1 h, and everything is left to stand at room temperature for 8 h. The filtrate is filtered off with suction and concentrated by evaporation under reduced pressure, the residue taken up in dichloromethane and washed once with water, and the organic phase dried over sodium sulphate. After concentration by evaporation under reduced pressure, 4.3 g (63% of theory; purity by GC/MS: 74 area %) of a semicrystalline residue are obtained.

1. waiteverything is left
2. waitto stand at room temperature for 8 h
3. filtrationThe filtrate is filtered off with suction
4. concentrationconcentrated by evaporation under reduced pressure
5. washwashed once with water
6. dry with materialthe organic phase dried over sodium sulphate
7. concentrationAfter concentration
8. customby evaporation under reduced pressure, 4.3 g (63% of theory; purity by GC/MS: 74 area %) of a semicrystalline residue
9. customare obtained

ORD-Eintrag

ord-56c0a4b08e76451d8ee60e988ae8266a

Quelldatensatz

uspto-grants-2006_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07078527B2