Carbon Tetrachloride → HCID 22617184, compound

Temperature

80 °C

First, 31.4 g (120 mmol) of triphenylphosphine and 4.9 g (48 mmol) of triethylamine were added to 20 ml of carbon tetrachloride, to which 3.8 g (40 mmol) of difluoroacetic acid was added dropwise under ice cooling. After completion of the dropwise addition, the mixture was stirred under ice cooling for 10 minutes. Then, a solution of 9.2 g (40 mmol) of 2,6-dichloro-4-trifluoromethylaniline in 20 ml of carbon tetrachloride was added dropwise to the reaction mixture, which was heated at 80° C. for 6 hours. The reaction mixture was concentrated under reduced pressure, followed by addition of hexane, and undissolved matter was removed by filtration. The filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 6.0 g of N-(2,6-dichloro-4-trifluoromethylphenyl)-2,2-difluoroacetimidoyl chloride.

1. additionwas added dropwise under ice cooling
2. additionAfter completion of the dropwise addition
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additionfollowed by addition of hexane, and undissolved matter
5. customwas removed by filtration
6. concentrationThe filtrate was concentrated under reduced pressure

ORD record

ord-615f54005fb74b1b836e5c4847eff605

Source dataset

uspto-grants-2002_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06376710B2