1,4-dichlorobenzene

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 2-methyl-6-nitrobenzothiazole (0.36 g) was added ethyl iodide (1.5 ml) and dichlorobenzene (20 ml). The mixture was heated to 120° C. for 2 days and then allowed to cool to room temperature. Ethyl acetate was added and the resulting precipitate removed by filtration. Drying in a vacuum oven gave the desired material (80 mg). to cool to room temperature the resulting precipitate removed by filtration Drying in a vacuum oven

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 2,3,3-trimethylindolenine (1.59 g) was added 1-bromo-2-(2-methoxyethoxy)ethane (2.75 g) and dichlorobenzene (5 ml). The mixture was heated to 70° C. overnight. The volatiles were stripped and the material purified by HPLC. the material purified by HPLC

反応条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 2,3,3-trimethylindolenine (1.64 g) was added 3,5-dinitrobenzyl iodide (3.71 g) and dichlorobenzene (15 ml). After heating to 90° C. for 6 hours the mixture was allowed to cool and the resultant precipitate removed by filtration. The solid was washed with dichlorobenzene (2×10 ml) and ether (2×50 ml). The material was dried in a vacuum oven to give the product as a yellow solid (2.69 g). to cool the resultant precipitate removed by filtration The solid was washed with dichlorobenzene (2×10 ml) and ether (2×50 ml) The material was dried in a vacuum oven

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

実験手順: In the same apparatus and procedures as EXAMPLE 2 above, 17.35 g (118 mmol) of 1,4-dichlorobenzene and 0.47 g (3.5 mmol) of aluminum chloride were alkylated with 5.45 g (23.5 mmol) of (1,2-dichloroethyl)trichlorosilane for 20 min at 120° C. The aluminum chloride catalyst was quenched with POCl3 and then stirred for another 1 hour to complete the deactivation. Freshly distilled hexane (50 ml) was added to the reaction mixture and insoluble solids in hexane were filtered from the organic soultion. After hexane was distilled, the reaction products were vacuum distilled to give 4.56 g of [2,2-bis(2,5-dichlorophenyl)ethyl]trichlorosilane (bp; 161-163° C./0.5 torr, yield; 43%). The aluminum chloride catalyst was quenched with POCl3 Freshly distilled hexane (50 ml) was added to the reaction mixture and insoluble solids in hexane were filtered from the organic soultion After hexane was distilled distilled

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

実験手順: In the same apparatus and procedures as EXAMPLE 2 above, 14.70 g (100 mmol) of 1,4-dichlorobenzene and 0.027 g (1.0 mmol) of aluminum foil were alkylated with 4.98 g (21.4 mmol) of (2,2-dichloroethyl)trichlorosilane for 1 hour at 80° C. Freshly distilled hexane (50 ml) was added to the reaction mixture and insoluble solids in hexane were filtered from the organic soultion. After hexane and benzene were distilled, the reaction products were vacuum distilled to give 3.33 g of [2,2-bis(2,5-dichlorophenyl)ethyl]trichlorosilane (bp; 161-163° C./1 torr, yield; 59%). were filtered from the organic soultion After hexane and benzene were distilled distilled