反応 #4039130
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-873bf6236a5a4b60bd944045d710df09表示可能な構造データがありません
C(CO)CS(=O)(=O)N製品情報
3-hydroxypropane-1-sulfonamide (CAS 132115-62-9) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 10486918
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
7 反応 · 7 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-873bf6236a5a4b60bd944045d710df09反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In 12 ml of dimethylformamide was suspended 0.48 g of 60% sodium hydride in oil followed by addition of 0.835 g of 3-hydroxy-1-propanesulfonamide and the mixture was stirred under reduced pressure at room temperature for 30 minutes. Then, 0.928 g of 6-chloro[1,2,4]triazolo[1,5-b]pyridazine was added and the mixture was further stirred at room temperature for 18 hours. Following addition of 40 ml of ice water, the reaction mixture was adjusted to pH6 with 1N-hydrochloric acid then saturated with sodium chloride. The aqueous layer was extracted with tetrahydrofuran and the extract was dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was crystallized from ethyl ether. The washed crystals were recrystallized from hot methanol to provide 0.811 g of title compound. m.p. 145°-147° C. the mixture was further stirred at room temperature for 18 hours The aqueous layer was extracted with tetrahydrofuran the extract was dried over magnesium sulfate The solvent was distilled off under reduced pressure the resulting residue was crystallized from ethyl ether The washed crystals were recrystallized from hot methanol
ソース ID: ord-ef5441d25a9b42f7b19df8c1f2556881反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In 12 ml of dimethylformamide was suspended 0.48 g of 60% sodium hydride in oil followed by addition of 0.835 g of 3-hydroxy-1-propanesulfonamide and the mixture was stirred under reduced pressure at room temperature for 30 minutes. Then, 0.928 g of 6-chloro[1,2,4]triazolo[1,5-b]pyridazine was added and the mixture was further stirred at room temperature for 18 hours. Following addition of 40 ml of ice water, the reaction mixture was adjusted to pH6 with 1N-hydrochloric acid then saturated with sodium chloride. The aqueous layer was extracted with tetrahydrofuran and the extract was dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was crystallized from ethyl ether. The washed crystals were recrystallized from hot methanol to provide 0.811 g of title compound. m.p. 145°-147° C. the mixture was further stirred at room temperature for 18 hours The aqueous layer was extracted with tetrahydrofuran the extract was dried over magnesium sulfate The solvent was distilled off under reduced pressure the resulting residue was crystallized from ethyl ether The washed crystals were recrystallized from hot methanol
ソース ID: ord-ef5441d25a9b42f7b19df8c1f2556881反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In 12 ml of dimethylformamide was suspended 0.48 g of 60% sodium hydride in oil followed by addition of 0.835 g of 3-hydroxy-1-propanesulfonamide and the mixture was stirred under reduced pressure at room temperature for 30 minutes. Then, 0.928 g of 6-chloro[1,2,4]triazolo[1,5-b]pyridazine was added and the mixture was further stirred at room temperature for 18 hours. Following addition of 40 ml of ice water, the reaction mixture was adjusted to pH6 with 1N-hydrochloric acid then saturated with sodium chloride. The aqueous layer was extracted with tetrahydrofuran and the extract was dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was crystallized from ethyl ether. The washed crystals were recrystallized from hot methanol to provide 0.811 g of title compound. m.p. 145°-147° C. the mixture was further stirred at room temperature for 18 hours The aqueous layer was extracted with tetrahydrofuran the extract was dried over magnesium sulfate The solvent was distilled off under reduced pressure the resulting residue was crystallized from ethyl ether The washed crystals were recrystallized from hot methanol
ソース ID: ord-ef5441d25a9b42f7b19df8c1f2556881反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In 12 ml of dimethylformamide was suspended 0.48 g of 60% sodium hydride in oil followed by addition of 0.835 g of 3-hydroxy-1-propanesulfonamide and the mixture was stirred under reduced pressure at room temperature for 30 minutes. Then, 0.928 g of 6-chloro[1,2,4]triazolo[1,5-b]pyridazine was added and the mixture was further stirred at room temperature for 18 hours. Following addition of 40 ml of ice water, the reaction mixture was adjusted to pH6 with 1N-hydrochloric acid then saturated with sodium chloride. The aqueous layer was extracted with tetrahydrofuran and the extract was dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was crystallized from ethyl ether. The washed crystals were recrystallized from hot methanol to provide 0.811 g of title compound. m.p. 145°-147° C. the mixture was further stirred at room temperature for 18 hours The aqueous layer was extracted with tetrahydrofuran the extract was dried over magnesium sulfate The solvent was distilled off under reduced pressure the resulting residue was crystallized from ethyl ether The washed crystals were recrystallized from hot methanol
ソース ID: ord-ef5441d25a9b42f7b19df8c1f2556881反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-873bf6236a5a4b60bd944045d710df09反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In 12 ml of dimethylformamide was suspended 0.48 g of 60% sodium hydride in oil followed by addition of 0.835 g of 3-hydroxy-1-propanesulfonamide and the mixture was stirred under reduced pressure at room temperature for 30 minutes. Then, 0.928 g of 6-chloro[1,2,4]triazolo[1,5-b]pyridazine was added and the mixture was further stirred at room temperature for 18 hours. Following addition of 40 ml of ice water, the reaction mixture was adjusted to pH6 with 1N-hydrochloric acid then saturated with sodium chloride. The aqueous layer was extracted with tetrahydrofuran and the extract was dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was crystallized from ethyl ether. The washed crystals were recrystallized from hot methanol to provide 0.811 g of title compound. m.p. 145°-147° C. the mixture was further stirred at room temperature for 18 hours The aqueous layer was extracted with tetrahydrofuran the extract was dried over magnesium sulfate The solvent was distilled off under reduced pressure the resulting residue was crystallized from ethyl ether The washed crystals were recrystallized from hot methanol
ソース ID: ord-ef5441d25a9b42f7b19df8c1f2556881PubChem References
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