1,1-dichloropropane

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A two-phase mixture of phenol (5 g, 53 mmol), dichloropropane (32 ml), tetrabutylammonium hydrogen sulphate (0.3 g, 1 mmol), and sodium hydroxide solution (25 ml, 3M) was refluxed for 3 h. The organic layer was separated, dried (MgSO4), washed through a plug of silica with dichloromethane (200 ml), and concentrated in vacuo. The residues were distilled to give the title compound as a colourless, viscous oil (8.0 g, 88%) bp 110° C. at 0.1 mm Hg. NMR (CDCl3, 250 MHz) δ=2.26 (2H,q,J=6 Hz), 3.77 (2H,t,J=6 Hz), 4.13 (2H,t,J=6 Hz), 6.90-7.00 (3H,m), 7.26-7.34 (2H,m). was refluxed for 3 h The organic layer was separated dried (MgSO4) washed through a plug of silica with dichloromethane (200 ml) concentrated in vacuo The residues were distilled

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

実験手順: A two-phase mixture of phenol (5 g, 53 mmol), dichloropropane (32 ml), tetrabutylammonium hydrogen sulphate (0.3 g, 1 mmol), and sodium hydroxide solution (25 ml, 3M) was refluxed for 3 h. The organic layer was separated, dried (MgSO4), washed through a plug of silica with dichloromethane (200 ml), and concentrated in vacuo. The residues were distilled to give the title compound as a colourless, viscous oil (8.0 g, 88%) bp 110° C. at 0.1 mm Hg. NMR (CDCl3, 250 MHz) δ=2.26 (2H,q,J=6 Hz), 3.77 (2H,t,J=6 Hz), 4.13 (2H,t,J=6 Hz), 6.90-7.00 (3H,m), 7.26-7.34 (2H,m). was refluxed for 3 h The organic layer was separated dried (MgSO4) washed through a plug of silica with dichloromethane (200 ml) concentrated in vacuo The residues were distilled

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

実験手順: In the present process, dichloropropane is converted to a chlorinated alkene, e.g., TCPE, using a series of consecutive chlorination and dehydrochlorination steps. In one exemplary embodiment, PDC is fed to a liquid phase chlorination reactor, e.g., such as a batch or continuous stirred tank autoclave reactor with an internal cooling coil. A shell and multitube exchanger operating in plug flow, followed by vapor liquid disengagement tank or vessel can also be used. Suitable reaction conditions include, e.g., a temperature of from 30° C. to 150° C., a pressure of from 100 kPa to 2000 kPa. The reaction is carried out in the presence of one or more regioselective catalysts that provide a regioselectivity to, e.g., 1,1,2-trichloropropane of at least 5:1 over other trichloropropane isomers. Suitable reaction conditions of from 30° C. to 150° C.

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

実験手順: In the present process, dichloropropane is converted to a chlorinated alkene, e.g., TCPE, using a series of consecutive chlorination and dehydrochlorination steps. In one exemplary embodiment, PDC is fed to a liquid phase chlorination reactor, e.g., such as a batch or continuous stirred tank autoclave reactor with an internal cooling coil. A shell and multitube exchanger operating in plug flow, followed by vapor liquid disengagement tank or vessel can also be used. Suitable reaction conditions include, e.g., a temperature of from 30° C. to 150° C., a pressure of from 100 kPa to 2000 kPa. The reaction is carried out in the presence of one or more regioselective catalysts that provide a regioselectivity to, e.g., 1,1,2-trichloropropane of at least 5:1 over other trichloropropane isomers. Suitable reaction conditions of from 30° C. to 150° C.

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A two-phase mixture of phenol (5 g, 53 mmol), dichloropropane (32 ml), tetrabutylammonium hydrogen sulphate (0.3 g, 1 mmol), and sodium hydroxide solution (25 ml, 3M) was refluxed for 3 h. The organic layer was separated, dried (MgSO4), washed through a plug of silica with dichloromethane (200 ml), and concentrated in vacuo. The residues were distilled to give the title compound as a colourless, viscous oil (8.0 g, 88%) bp 110° C. at 0.1 mm Hg. NMR (CDCl3, 250 MHz) δ=2.26 (2H,q,J=6 Hz), 3.77 (2H,t,J=6 Hz), 4.13 (2H,t,J=6 Hz), 6.90-7.00 (3H,m), 7.26-7.34 (2H,m). was refluxed for 3 h The organic layer was separated dried (MgSO4) washed through a plug of silica with dichloromethane (200 ml) concentrated in vacuo The residues were distilled

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

実験手順: In the present process, dichloropropane is converted to a chlorinated alkene, e.g., TCPE, using a series of consecutive chlorination and dehydrochlorination steps. In one exemplary embodiment, PDC is fed to a liquid phase chlorination reactor, e.g., such as a batch or continuous stirred tank autoclave reactor with an internal cooling coil. A shell and multitube exchanger operating in plug flow, followed by vapor liquid disengagement tank or vessel can also be used. Suitable reaction conditions include, e.g., a temperature of from 30° C. to 150° C., a pressure of from 100 kPa to 2000 kPa. The reaction is carried out in the presence of one or more regioselective catalysts that provide a regioselectivity to, e.g., 1,1,2-trichloropropane of at least 5:1 over other trichloropropane isomers. Suitable reaction conditions of from 30° C. to 150° C.