6-chloro-5-(2-chloroethyl)-1,3-dihydroindol-2-one

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:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 100 g of 5-(2-chloroethyl)-6-chlorooxindole, 95.2 g of 3-(1-piperazinyl)-1,2-benzisothiazole, 92.1 g of sodium carbonate, 6.5 g of sodium iodide, 28 g of tetrabutylammonium bromide and 1000 ml of cyclohexane was refluxed until reaction completion as shown by thin layer chromatography. The reaction mass was cooled to 30° C. and the solid was filtered. 1000 ml of water was added to the wet compound and stirred for 95 minutes. The solid was filtered and washed with 100 ml water. To the wet compound, 1000 ml methanol was added and stirred for 2.5 to 3 hours at room temperature. The compound was filtered and washed with 200 ml of methanol and dried to afford 142.6 g of the title compound. was refluxed until reaction completion the solid was filtered 1000 ml of water was added to the wet compound The solid was filtered washed with 100 ml water To the wet compound, 1000 ml methanol was added stirred for 2.5 to 3 hours at room temperature The compound was filtered washed with 200 ml of methanol dried

反応条件: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 100 g of 5-(2-chloroethyl)-6-chlorooxindole, 95.2 g of 3-(1-piperazinyl)-1,2-benzisothiazole, 92.1 g of sodium carbonate, 6.5 g of sodium iodide, 28 g of tetrabutylammonium bromide and 1000 ml of cyclohexane was refluxed until reaction completion as shown by thin layer chromatography. The reaction mass was cooled to 30° C. and the solid was filtered. 1000 ml of water was added to the wet compound and stirred for 95 minutes. The solid was filtered and washed with 100 ml water. To the wet compound, 1000 ml methanol was added and stirred for 2.5 to 3 hours at room temperature. The compound was filtered and washed with 200 ml of methanol and dried to afford 142.6 g of the title compound. was refluxed until reaction completion the solid was filtered 1000 ml of water was added to the wet compound The solid was filtered washed with 100 ml water To the wet compound, 1000 ml methanol was added stirred for 2.5 to 3 hours at room temperature The compound was filtered washed with 200 ml of methanol dried

反応条件: temp:42.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 130 g of 5-(2-chloroacetyl)-6-chlorooxindole, 455 ml of trifluoroacetic acid and 148.6 g of triethylsilane was maintained at a temperature of about 40-45° C. for 7 hours. The reaction mass was filtered at −5 to 0° C. after maintaining for 1 to 2 hours at the same temperature. The compound was washed with 130 ml of water and further slurried in 650 ml of water. After separation from the water, it was then dried to yield 113 g of the title compound. The reaction mass was filtered at −5 to 0° C. after maintaining for 1 to 2 hours at the same temperature The compound was washed with 130 ml of water and further slurried in 650 ml of water After separation from the water, it was then dried