1-(4-氟苯基磺酰)吡咯啉

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: To a solution of pyrolidine (17 mL, 237 mmol) in 20 mL of H2O at room temperature was added p-flourobenzenesulfonyl chloride (15 g, 79 mmol) in portions over a 5 minute period. After 1 hour, the solution was diluted with 100 mL of H2O and extracted with ethyl acetate (3×50 mL). The organic was dried (Na2SO4) and concentrated in vacuo to give 12.3 g (72%) of 4-(pyrrolidinosulfonyl)-flourobenzene as a colorless oil that solidified on standing. This material was used in the following reaction without further purification. MS. extracted with ethyl acetate (3×50 mL) The organic was dried (Na2SO4) concentrated in vacuo

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

实验步骤: To a solution of pyrolidine (17 mL, 237 mmol) in 20 mL of H2O at room temperature was added p-flourobenzenesulfonyl chloride (15 g, 79 mmol) in portions over a 5 minute period. After 1 hour, the solution was diluted with 100 mL of H2O and extracted with ethyl acetate (3×50 mL). The organic was dried (Na2SO4) and concentrated in vacuo to give 12.3 g (72%) of 4-(pyrrolidinosulfonyl)-flourobenzene as a colorless oil that solidified on standing. This material was used in the following reaction without further purification. MS. extracted with ethyl acetate (3×50 mL) The organic was dried (Na2SO4) concentrated in vacuo

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

实验步骤: To a solution of pyrolidine (17 mL, 237 mmol) in 20 mL of H2O at room temperature was added p-flourobenzenesulfonyl chloride (15 g, 79 mmol) in portions over a 5 minute period. After 1 hour, the solution was diluted with 100 mL of H2O and extracted with ethyl acetate (3×50 mL). The organic was dried (Na2SO4) and concentrated in vacuo to give 12.3 g (72%) of 4-(pyrrolidinosulfonyl)-flourobenzene as a colorless oil that solidified on standing. This material was used in the following reaction without further purification. MS. extracted with ethyl acetate (3×50 mL) The organic was dried (Na2SO4) concentrated in vacuo

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

实验步骤: To a solution of pyrolidine (17 mL, 237 mmol) in 20 mL of H2O at room temperature was added p-flourobenzenesulfonyl chloride (15 g, 79 mmol) in portions over a 5 minute period. After 1 hour, the solution was diluted with 100 mL of H2O and extracted with ethyl acetate (3×50 mL). The organic was dried (Na2SO4) and concentrated in vacuo to give 12.3 g (72%) of 4-(pyrrolidinosulfonyl)flourobenzene as a colorless oil that solidified on standing. This material was used in the following reaction without further purification. MS. extracted with ethyl acetate (3×50 mL) The organic was dried (Na2SO4) concentrated in vacuo

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

实验步骤: To a solution of pyrolidine (17 mL, 237 mmol) in 20 mL of H2O at room temperature was added p-flourobenzenesulfonyl chloride (15 g, 79 mmol) in portions over a 5 minute period. After 1 hour, the solution was diluted with 100 mL of H2O and extracted with ethyl acetate (3×50 mL). The organic was dried (Na2SO4) and concentrated in vacuo to give 12.3 g (72%) of 4-(pyrrolidinosulfonyl)flourobenzene as a colorless oil that solidified on standing. This material was used in the following reaction without further purification. MS. extracted with ethyl acetate (3×50 mL) The organic was dried (Na2SO4) concentrated in vacuo

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

实验步骤: To a solution of pyrolidine (17 mL, 237 mmol) in 20 mL of H2O at room temperature was added p-flourobenzenesulfonyl chloride (15 g, 79 mmol) in portions over a 5 minute period. After 1 hour, the solution was diluted with 100 mL of H2O and extracted with ethyl acetate (3×50 mL). The organic was dried Na2SO4) and concentrated in vacuo to give 12.3 g (72%) of 4-(pyrrolidinosulfonyl)flourobenzene as a colorless oil that solidified on standing. This material was used in the following reaction without further purification. MS. extracted with ethyl acetate (3×50 mL) concentrated in vacuo

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

实验步骤: To a solution of pyrolidine (17 mL, 237 mmol) in 20 mL of H2O at room temperature was added p-flourobenzenesulfonyl chloride (15 g, 79 mmol) in portions over a 5 minute period. After 1 hour, the solution was diluted with 100 mL of H2O and extracted with ethyl acetate (3×50 mL). The organic was dried (Na2SO4) and concentrated in vacuo to give 12.3 g (72%) of 4-(pyrrolidinosulfonyl)-flourobenzene as a colorless oil that solidified on standing. This material was used in the following reaction without further purification. MS. extracted with ethyl acetate (3×50 mL) The organic was dried (Na2SO4) concentrated in vacuo

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 5-bromo-3-pyridinol (2.61 g, 15 mmol), dimethylacetamide (50 mL), 1-((4-fluorophenyl)sulfonyl)pyrrolidine (5.8 g, 25 mmol) and potassium carbonate (4.1 g, 30 mmol) was heated at 120° C. for 18 h, then cooled to room temperature and concentrated by rotary evaporation. The residue was dissolved in ethyl acetate (200 mL) and the organic phase washed with water (3×100 mL) and brine (100 mL), then dried (MgSO4), filtered and concentrated by rotary evaporation. The crude product was purified by column chromatography, eluting with ethyl acetate/cyclohexane (20/80, v/v). Selected fractions containing the product were concentrated via rotary evaporation to give 3.4 g (59%) of a red solid (m.p. 148° C.) cooled to room temperature concentrated by rotary evaporation The residue was dissolved in ethyl acetate (200 mL) the organic phase washed with water (3×100 mL) and brine (100 mL) dried (MgSO4) filtered concentrated by rotary evaporation The crude product was purified by column chromatography eluting with ethyl acetate/cyclohexane (20/80 Selected fractions containing the product were concentrated via rotary evaporation

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 5-bromo-3-pyridinol (2.61 g, 15 mmol), dimethylacetamide (50 mL), 1-((4-fluorophenyl)sulfonyl)pyrrolidine (5.8 g, 25 mmol) and potassium carbonate (4.1 g, 30 mmol) was heated at 120° C. for 18 h, then cooled to room temperature and concentrated by rotary evaporation. The residue was dissolved in ethyl acetate (200 mL) and the organic phase washed with water (3×100 mL) and brine (100 mL), then dried (MgSO4), filtered and concentrated by rotary evaporation. The crude product was purified by column chromatography, eluting with ethyl acetate/cyclohexane (20/80, v/v). Selected fractions containing the product were concentrated via rotary evaporation to give 3.4 g (59%) of a red solid (m.p. 148° C.) cooled to room temperature concentrated by rotary evaporation The residue was dissolved in ethyl acetate (200 mL) the organic phase washed with water (3×100 mL) and brine (100 mL) dried (MgSO4) filtered concentrated by rotary evaporation The crude product was purified by column chromatography eluting with ethyl acetate/cyclohexane (20/80 Selected fractions containing the product were concentrated via rotary evaporation

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

实验步骤: To a solution of pyrrolidine (17 mL, 237 mmol) in 20 mL of H2O at room temperature was added p-flourobenzenesulfonyl chloride (15 g, 79 mmol) in portions over a 5 minute period. After 1 hour, the solution was diluted with 100 mL of H2O and extracted with ethyl acetate (3×50 mL). The organic was dried (Na2SO4) and concentrated in vacuo to give 12.3 g (72%) of 4-(pyrrolidinosulfonyl)-flourobenzene as a colorless oil that solidified on standing. This material was used in the following reaction without further purification. MS. extracted with ethyl acetate (3×50 mL) The organic was dried (Na2SO4) concentrated in vacuo