prop-2-enyl 2-chloro-2,2-difluoroacetate

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 100.0 g (0.59 mol) of allyl chlorodifluoroacetate, 42.2 g (0.65 mol) of zinc dust (activated according to Fieser & Fieser), 96.7 g (0.88 mol) of trimethylchlorosilane and 400 ml of absolute acetonitrile are introduced together into a glass autoclave, a spatula tip of iodine is added and the mixture is heated for 48 hours at 100° C. The zinc salt which has precipitated is filtered off, the filtrate is hydrolysed with H2O and rendered basic with 2N NaOH. The dark brown aqueous phase, extracted with pentane, is acidified with half-concentrated HCl, and the product is extracted with ethyl acetate. After the organic phase has been dried over MgSO4 and evaporated in a rotary evaporator (RE), the residue is distilled in vacuo. Yield: 59.4 g (74%) of a colourless oil of boiling point 73°-75° C./15.6 mbar. The zinc salt which has precipitated is filtered off The dark brown aqueous phase, extracted with pentane the product is extracted with ethyl acetate After the organic phase has been dried over MgSO4 evaporated in a rotary evaporator (RE), the residue is distilled in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 1.5 liter sulfonation flask with a water separator, 294.0 g (2.25 mol) of chlorodifluoroacetic acid (pure, from Fluka AG) and 228.0 g (3.93 mol) of allyl alcohol are dissolved in 1 liter of chloroform and kept under reflux for 17 hours in the presence of 11.25 g of p-toluenesulfonic acid (0.06 mol), 41 ml of H2O separating out. The yellow reaction solution is washed twice with H2O and 3 times with saturated aqueous NaHCO3 solution, dried over MgSO4 and distilled under normal pressure through a Vigreux column. Yield: 306.0 g (80%) of a colourless oil of boiling point 98°-100° C./988 mbar. The yellow reaction solution is washed twice with H2O and 3 times with saturated aqueous NaHCO3 solution dried over MgSO4 distilled under normal pressure through a Vigreux column

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 100.0 g (0.59 mol) of allyl chlorodifluoroacetate, 42.2 g (0.65 mol) of zinc dust (activated according to Fieser & Fieser), 96.7 g (0.88 mol) of trimethylchlorosilane and 400 ml of absolute acetonitrile are introduced together into a glass autoclave, a spatula tip of iodine is added and the mixture is heated for 48 hours at 100° C. The zinc salt which has precipitated is filtered off, the filtrate is hydrolysed with H2O and rendered basic with 2N NaOH. The dark brown aqueous phase, extracted with pentane, is acidified with half-concentrated HCl, and the product is extracted with ethyl acetate. After the organic phase has been dried over MgSO4 and evaporated in a rotary evaporator (RE), the residue is distilled in vacuo. Yield: 59.4 g (74%) of a colourless oil of boiling point 73°-75° C./15.6 mbar. The zinc salt which has precipitated is filtered off The dark brown aqueous phase, extracted with pentane the product is extracted with ethyl acetate After the organic phase has been dried over MgSO4 evaporated in a rotary evaporator (RE), the residue is distilled in vacuo

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 100.0 g (0.59 mol) of allyl chlorodifluoroacetate, 42.2 g (0.65 mol) of zinc dust (activated according to Fieser & Fieser), 96.7 g (0.88 mol) of trimethylchlorosilane and 400 ml of absolute acetonitrile are introduced together into a glass autoclave, a spatula tip of iodine is added and the mixture is heated for 48 hours at 100° C. The zinc salt which has precipitated is filtered off, the filtrate is hydrolysed with H2O and rendered basic with 2N NaOH. The dark brown aqueous phase, extracted with pentane, is acidified with half-concentrated HCl, and the product is extracted with ethyl acetate. After the organic phase has been dried over MgSO4 and evaporated in a rotary evaporator (RE), the residue is distilled in vacuo. Yield: 59.4 g (74%) of a colourless oil of boiling point 73°-75° C./15.6 mbar. The zinc salt which has precipitated is filtered off The dark brown aqueous phase, extracted with pentane the product is extracted with ethyl acetate After the organic phase has been dried over MgSO4 evaporated in a rotary evaporator (RE), the residue is distilled in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 1.5 liter sulfonation flask with a water separator, 294.0 g (2.25 mol) of chlorodifluoroacetic acid (pure, from Fluka AG) and 228.0 g (3.93 mol) of allyl alcohol are dissolved in 1 liter of chloroform and kept under reflux for 17 hours in the presence of 11.25 g of p-toluenesulfonic acid (0.06 mol), 41 ml of H2O separating out. The yellow reaction solution is washed twice with H2O and 3 times with saturated aqueous NaHCO3 solution, dried over MgSO4 and distilled under normal pressure through a Vigreux column. Yield: 306.0 g (80%) of a colourless oil of boiling point 98°-100° C./988 mbar. The yellow reaction solution is washed twice with H2O and 3 times with saturated aqueous NaHCO3 solution dried over MgSO4 distilled under normal pressure through a Vigreux column

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 1.5 liter sulfonation flask with a water separator, 294.0 g (2.25 mol) of chlorodifluoroacetic acid (pure, from Fluka AG) and 228.0 g (3.93 mol) of allyl alcohol are dissolved in 1 liter of chloroform and kept under reflux for 17 hours in the presence of 11.25 g of p-toluenesulfonic acid (0.06 mol), 41 ml of H2O separating out. The yellow reaction solution is washed twice with H2O and 3 times with saturated aqueous NaHCO3 solution, dried over MgSO4 and distilled under normal pressure through a Vigreux column. Yield: 306.0 g (80%) of a colourless oil of boiling point 98°-100° C./988 mbar. The yellow reaction solution is washed twice with H2O and 3 times with saturated aqueous NaHCO3 solution dried over MgSO4 distilled under normal pressure through a Vigreux column

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 100.0 g (0.59 mol) of allyl chlorodifluoroacetate, 42.2 g (0.65 mol) of zinc dust (activated according to Fieser & Fieser), 96.7 g (0.88 mol) of trimethylchlorosilane and 400 ml of absolute acetonitrile are introduced together into a glass autoclave, a spatula tip of iodine is added and the mixture is heated for 48 hours at 100° C. The zinc salt which has precipitated is filtered off, the filtrate is hydrolysed with H2O and rendered basic with 2N NaOH. The dark brown aqueous phase, extracted with pentane, is acidified with half-concentrated HCl, and the product is extracted with ethyl acetate. After the organic phase has been dried over MgSO4 and evaporated in a rotary evaporator (RE), the residue is distilled in vacuo. Yield: 59.4 g (74%) of a colourless oil of boiling point 73°-75° C./15.6 mbar. The zinc salt which has precipitated is filtered off The dark brown aqueous phase, extracted with pentane the product is extracted with ethyl acetate After the organic phase has been dried over MgSO4 evaporated in a rotary evaporator (RE), the residue is distilled in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 1.5 liter sulfonation flask with a water separator, 294.0 g (2.25 mol) of chlorodifluoroacetic acid (pure, from Fluka AG) and 228.0 g (3.93 mol) of allyl alcohol are dissolved in 1 liter of chloroform and kept under reflux for 17 hours in the presence of 11.25 g of p-toluenesulfonic acid (0.06 mol), 41 ml of H2O separating out. The yellow reaction solution is washed twice with H2O and 3 times with saturated aqueous NaHCO3 solution, dried over MgSO4 and distilled under normal pressure through a Vigreux column. Yield: 306.0 g (80%) of a colourless oil of boiling point 98°-100° C./988 mbar. The yellow reaction solution is washed twice with H2O and 3 times with saturated aqueous NaHCO3 solution dried over MgSO4 distilled under normal pressure through a Vigreux column