2-chloro-1,1-difluoroethene

Conditions: temp:300.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 600 cc "Hastelloy" C Parr autoclave was added 607.6 gm (4 mole) CsF, 58.1 gm (1 mole) KF and 80 gm (4 mole) HF. The reactor was then warmed to 300° C. with a back pressure regulator set at 300 psig. Liquid HCFC-133a was then continuously fed to the agitated molten mixture at a constant rate of 0.0192 mole per minute by means of a high pressure liquid chromatography (HPLC) pump. Gas samples were then collected continuously as pressure greater than 300 psig was vented by the back pressure regulator. The reactor effluent was sampled automatically and analyzed by gas chromatography (GC). The conversion during the first 1.2 hours was 59%; dropping slowly to 27% over the next 1.2 hours. Selectivity to HFC-134a was greater than 99% over the entire run. HCFC-1122 is also formed by elimination of HF from HCFC-133a and constituted the remaining less than 1%. Gas samples were then collected continuously as pressure greater than 300 psig The reactor effluent was sampled automatically during the first 1.2 hours dropping slowly to 27% over the next 1.2 hours

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: N-Boc-L-cysteine is reacted with 2-chloro-1,1-difluoro-ethene in the same manner as described in J. Chem, Res. Miniprint 12, 1990; p 2868 to form N-Boc-S-(2-chloro-1,1-di fluoroethyl)-L-cysteine. N-Boc-S-(2-chloro-1,1-difluoroethyl)-L-cysteine is reacted with potassium phthalimide in DMF at 100° C. to form the phthalimide. The phthalimide is treated with hydrazine in ethanol to form the amine. The amine is treated with ethyl acetimidate hydrochloride to form the amidine. This material is purified via C-18 chromatography to afford the Boc compound. The Boc group is removed with HCl/dioxane (4 N) in acetic acid to afford the title compound.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: reacting 1,1,1-trifluorochloroethane from the first reaction zone with hydrogen fluoride in the gas phase in the presence of a fluorination catalyst to obtain 1,1,1,2-tetrafluoroethane and by-product 1,1-difluorochloroethylene in the second reaction zone,

Conditions: temp:300.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 600 cc "Hastelloy" C Parr autoclave was added 607.6 gm (4 mole) CsF, 58.1 gm (1 mole) KF and 80 gm (4 mole) HF. The reactor was then warmed to 300° C. with a back pressure regulator set at 300 psig. Liquid HCFC-133a was then continuously fed to the agitated molten mixture at a constant rate of 0.0192 mole per minute by means of a high pressure liquid chromatography (HPLC) pump. Gas samples were then collected continuously as pressure greater than 300 psig was vented by the back pressure regulator. The reactor effluent was sampled automatically and analyzed by gas chromatography (GC). The conversion during the first 1.2 hours was 59%; dropping slowly to 27% over the next 1.2 hours. Selectivity to HFC-134a was greater than 99% over the entire run. HCFC-1122 is also formed by elimination of HF from HCFC-133a and constituted the remaining less than 1%. Gas samples were then collected continuously as pressure greater than 300 psig The reactor effluent was sampled automatically during the first 1.2 hours dropping slowly to 27% over the next 1.2 hours