5-chloro-4H-1,4-benzothiazin-3-one

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The zinc salt (2.0 g) of 2-amino-3-chlorothiophenol was suspended in water (30 ml), and bromoacetic acid (1.6 g) was added thereto, followed by stirring at 70° C. for 3 hours. The precipitated crystals were filtered, washed with water and dried to obtain 1.8 g of the objective 5-chloro-2,3-dihydro-1,4-benzothiazine-3-one (m.p. 160°-161° C.). The precipitated crystals were filtered washed with water dried

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

実験手順: 2-Amino-3-chlorothiophenol (2.5 g) was dissolved in a solution of sodium hydroxide (690 mg) in water (40 ml), and bromoacetic acid (2.4 g) was added thereto with stirring. After stirring at 70° C. for 3 hours, the precipitated crystals were filtered, washed with water and dried to obtain 2.98 g of the objective 5-chloro-2,3-dihydro-1,4-benzothiazine-3-one (m.p. 160°-161° C.) was added After stirring at 70° C. for 3 hours the precipitated crystals were filtered washed with water dried

反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5-Chloro-2,3-dihydro-1,4-benzothiazine-3-one (2.0 g) and phosphorus pentasulfide (2.0 g) were added to pyridine (5 ml), followed by stirring at 120° C. for 20 minutes. The reaction mixture was then poured into a dilute hydrochloric acid (50 ml), and the precipitated crystals were filtered, washed with water, dried and recrystallized from ethanol to obtain 1.9 g of the objective 5-chloro-2,3-dihydro-1,4-benzothiazine-3-thione (m.p. 138°-140° C.). the precipitated crystals were filtered washed with water dried recrystallized from ethanol

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The zine salt (2.0 g) of 2-amino-3-chlorothiophenol was suspended in water (30 ml), and bromoacetic acid (1.6 g) was added thereto, followed by stirring at 70° C. for 3 hours. The precipitated crystals were filtered, washed with water and dried to obtain 1.8 g of the objective 5-chloro-2,3-dihydro-1,4-benzothiazine-3-one (m.p. 160°-161° C.). The precipitated crystals were filtered washed with water dried

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

実験手順: 2-Amino-3-chlorothiophenol (2.5 g) was dissolved in a solution of sodium hydroxide (690 mg) in water (40 ml), and bromoacetic acid (2.4 g) was added thereto with stirring. After stirring at 70° C. for 3 hours, the precipitated crystals were filtered, washed with water and dried to obtain 2.98 g of the objective 5-chloro-2,3-dihydro-1,4-benzothiazine-3-one (m.p. 160°-161° C.). was added After stirring at 70° C. for 3 hours the precipitated crystals were filtered washed with water dried

反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 5-Chloro-2,3-dihydro-1,4-benzothiazine-3-one (2.0 g) and phosphorus pentasulfide (2.0 g) were added to pyridine (5 ml), followed by stirring at 120° C. for 20 minutes. The reaction mixture was then poured into a dilute hydrochloric acid (50 ml), and the precipitated crystals were filtered, washed with water, dried and recrystallized from ethanol to obtain 1.9 g of the objective 5-chloro-2,3-dihydro-1,4-benzothiazine-3-thione (m.p. 138°-140° C.). the precipitated crystals were filtered washed with water dried recrystallized from ethanol