4-(2-bromoethyl)benzene-1-sulfonyl chloride

反应条件: temp:35.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3-Methyl-2-pyridinamine (431 g, 4.0 mol) was dissolved in dichloromethane (700 ml) and 4-(2-bromoethyl)benzenesulfonyl chloride (340 g, 1.33 mol) was added at room temperature. After 1 h at 20° C., the solution was heated to 35° C. for 2 h. Excess dilute hydrochloric acid was added and the phases separated. After washing once with water, the organic phase was dried with MgSO4 and treated with decolorizing carbon. The solvent was evaporated and warm methanol added to the residue, which crystallized. The material was collected and recrystallized from toluene. Yield 178 g. A further crop of 36 g was obtained by workup of the mother liquor. Total yield 45%. the phases separated After washing once with water the organic phase was dried with MgSO4 treated with decolorizing carbon The solvent was evaporated warm methanol added to the residue, which crystallized The material was collected recrystallized from toluene A further crop of 36 g was obtained by workup of the mother liquor

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-bromoethylbenzene (10.0 g; 54 mmol) in 16 ml of chloroform placed at a temperature of 0° C. was added dropwise a solution of chlorosulfonic acid (162 mmol, 18.87 g; 10.82 ml) in 11 ml of chloroform. After 15 minutes at 0° C., the reaction was maintained at room temperature for 3 hours. The reaction mixture was poured onto ice, and the aqueous phase was extracted with chloroform. The combined organic phases were washed with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was evaporated off to give 12.34 g of crude product, which was purified by chromatography on a column of silica, eluting with chloroform (76% yield). The product obtained was used for the following reaction without further purification. placed at a temperature of 0° C. The reaction mixture was poured onto ice the aqueous phase was extracted with chloroform The combined organic phases were washed with saturated sodium chloride solution dried over anhydrous sodium sulfate The solvent was evaporated off

反应条件: temp:35.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3-Methyl-2-pyridinamine (431 g, 4.0 mol) was dissolved in dichloromethane (700 ml) and 4-(2-bromoethyl)benzenesulfonyl chloride (340 g, 1.33 mol) was added at room temperature. After 1 h at 20° C., the solution was heated to 35° C. for 2 h. Excess dilute hydrochloric acid was added and the phases separate& After washing once with water, the organic phase was dried with MgSO4 and treated with decolorizing carbon. The solvent was evaporated and warm methanol added to the residue, which crystallized. The material was collected and recrystallized from toluene. Yield 178 g. A further crop of 36 g was obtained by workup of the mother liquor. Total yield 45%. the phases separate& After washing once with water the organic phase was dried with MgSO4 treated with decolorizing carbon The solvent was evaporated warm methanol added to the residue, which crystallized The material was collected recrystallized from toluene A further crop of 36 g was obtained by workup of the mother liquor

反应条件: temp:35.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3-Methyl-2-pyridinamine (431 g, 4.0 mol) was dissolved in dichloromethane (700 ml) and 4-(2-bromoethyl)benzenesulfonyl chloride (340 g, 1.33 mol) was added at room temperature. After 1 h at 20° C., the solution was heated to 35° C. for 2 h. Excess dilute hydrochloric acid was added and the phases separated. After washing once with water, the organic phase was dried with MgSO4 and treated with decolorizing carbon. The solvent was evaporated and warm methanol added to the residue, which crystallized. The material was collected and recrystallized from toluene. Yield 178 g. A further crop of 36 g was obtained by workup of the mother liquor. Total yield 45%. the phases separated After washing once with water the organic phase was dried with MgSO4 treated with decolorizing carbon The solvent was evaporated warm methanol added to the residue, which crystallized The material was collected recrystallized from toluene A further crop of 36 g was obtained by workup of the mother liquor

反应条件: temp:35.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3-Methyl-2-pyridinamine (431 g, 4.0 mol) was dissolved in dichloromethane (700 ml) and 4-(2-bromoethyl)benzenesulfonyl chloride (340 g, 1.33 mol) was added at room temperature. After 1 h at 20° C., the solution was heated to 35° C. for 2 h. Excess dilute hydrochloric acid was added and the phases separated. After washing once with water, the organic phase was dried with MgSO4 and treated with decolorizing carbon. The solvent was evaporated and warm methanol added to the residue, which crystallized. The material was collected and recrystallized from toluene. Yield 178 g. A further crop of 36 g was obtained by workup of the mother liquor. Total yield 45%. the phases separated After washing once with water the organic phase was dried with MgSO4 treated with decolorizing carbon The solvent was evaporated warm methanol added to the residue, which crystallized The material was collected recrystallized from toluene A further crop of 36 g was obtained by workup of the mother liquor