sulfo acetate

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

実験手順: The title compound was prepared using a procedure similar to the procedure used to prepare Example 5. The 5-acetoxy-2-naphthalenesulfonyl chloride was prepared by acylating 0.30 g (1.25 mmol) of 5-hydroxy-2-naphthalenesulfonic acid with acetic anhydride and pyridine. The acetoxysulfonic acid was then treated with POCl3 yielding an orange oil, 0.26 g. The oil was reacted with 0.12 g (0.96 mmol) of the azabicyclononane in CHCl3 solution. The usual work-up gave 270 mg of a green oil. Purification by chromatotron using 8/1/1 hexane/acetone/chloroform gave a yellow oil, 75 mg (22% yield): 1H NMR (CDCl3): 8.34 (d, J=1.5, 1 H, H1), 7.99 (d, J=8.9, 1 H, H3), 7.87 (d, J=8.4, 1 H, H6), 7.78 (d, J=8.9, 1 H, H4), 7.60 (t, J=8.0, 1 H, H7), 7.40 (d, J=7.6, 1 H, H8), 3.29 (d, J=4.2, 4 H, N(CH2R)2), 2.50 (s, 3 H, CH3), 2.08 (s, 2 H, N(CH2CHR)2) 1.74-1.61 (m, 8 H, alkyl H's). to prepare Example 5

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

実験手順: 2,5-dichloro-4′-phenoxybenzophenone (A, 137.3 g, 400 mmol) was put in a 3 L three-necked flask equipped with a stirring device and cooling tube, and 500 mL of 1,2-dichloroethane (1,2-DCE) was added and dissolved. Furthermore, 2 M of acetyl sulfuric acid solution prepared by mixing 56 mL of concentrated sulfuric acid, 152 mL of acetic anhydride, and 400 mL of 1,2-DCE, was added to the flask while stirring, and the reaction was performed in an oil bath at 60° C. After the predetermined period, 300 mL of 1-propanol was added to stop the reaction. Next, the reaction liquid was concentrated to a volume of 400 mL, and NaOH aqueous solution (120 g (3 mol)/water 400 mL) was added. The remaining 1,2-DCE in the reaction liquid was removed by azeotropic distillation, and a transparent light yellow solution was obtained. The light yellow solution was cooled, and deposition was filtered. The deposition was dried in a vacuum at 70° C. to obtain a white fine powder of 4-[4-(2,5-dichlorobenzoyl)phenoxy]benzene sulfonic acid sodium salt (A—SO3Na) shown in Chemical Formula 3. The crude crystal was used in the next process without being purified. equipped with a stirring device cooling tube dissolved was added to the flask the reaction was performed in an oil bath at 60° C the reaction Next, the reaction liquid was added was removed by azeotropic distillation a transparent light yellow solution was obtained The light yellow solution was cooled deposition was filtered The deposition was dried in a vacuum at 70° C.

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

実験手順: 2,5-dichloro-4′-phenoxybenzophenone (A, 137.3 g, 400 mmol) was put in a 3 L three-necked flask equipped with a stirring device and cooling tube, and 500 mL of 1,2-dichloroethane (1,2-DCE) was added and dissolved. Furthermore, 2 M of acetyl sulfuric acid solution prepared by mixing 56 mL of concentrated sulfuric acid, 152 mL of acetic anhydride, and 400 mL of 1,2-DCE, was added to the flask while stirring, and the reaction was performed in an oil bath at 60° C. After the predetermined period, 300 mL of 1-propanol was added to stop the reaction. Next, the reaction liquid was concentrated to a volume of 400 mL, and NaOH aqueous solution (120 g (3 mol)/water 400 mL) was added. The remaining 1,2-DCE in the reaction liquid was removed by azeotropic distillation, and a transparent light yellow solution was obtained. The light yellow solution was cooled, and deposition was filtered. The deposition was dried in a vacuum at 70° C. to obtain a white fine powder of 4-[4-(2,5-dichlorobenzoyl)phenoxy]benzene sulfonic acid sodium salt (A—SO3Na) shown in Chemical Formula 3. The crude crystal was used in the next process without being purified. equipped with a stirring device cooling tube dissolved was added to the flask the reaction was performed in an oil bath at 60° C the reaction Next, the reaction liquid was added was removed by azeotropic distillation a transparent light yellow solution was obtained The light yellow solution was cooled deposition was filtered The deposition was dried in a vacuum at 70° C.

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

実験手順: The title compound was prepared using a procedure similar to the procedure used to prepare Example 5. The 5-acetoxy-2-naphthalenesulfonyl chloride was prepared by acylating 0.30 g (1.25 mmol) of 5-hydroxy-2-naphthalenesulfonic acid with acetic anhydride and pyridine. The acetoxysulfonic acid was then treated with POCl3 yielding an orange oil, 0.26 g. The oil was reacted with 0.12 g (0.96 mmol) of the azabicyclononane in CHCl3 solution. The usual work-up gave 270 mg of a green oil. Purification by chromatotron using 8/1/1 hexane/acetone/chloroform gave a yellow oil, 75 mg (22% yield): 1H NMR (CDCl3): 8.34 (d, J=1.5, 1 H, H1), 7.99 (d, J=8.9, 1 H, H3), 7.87 (d, J=8.4, 1 H, H6), 7.78 (d, J=8.9, 1 H, H4), 7.60 (t, J=8.0, 1 H, H7), 7.40 (d, J=7.6, 1 H, H8), 3.29 (d, J=4.2, 4 H, N(CH2R)2), 2.50 (s, 3 H, CH3), 2.08 (s, 2 H, N(CH2CHR)2) 1.74-1.61 (m, 8 H, alkyl H's). to prepare Example 5