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

温度

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レコード

ord-a799ba5cb39d4e0b8ea74c4cb6b7d939

出典データセット

uspto-grants-2008_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07439408B2