2-chloro-N-hydroxybenzenecarboximidoyl chloride

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

実験手順: A solution of triethylamine (48 mL) in diethyl ether (0.5 L) was added over two hours to a 0° C. solution of the compound prepared in Example 5 (50.0 g) and propargyl alcohol (31 mL) in diethyl ether (1.2 L). The reaction was stirred at room temperature overnight, washed with water, dried over anhydrous magnesium sulfate and concentrated to obtain the title compound (50.0 g) having the following physical data. washed with water dried over anhydrous magnesium sulfate concentrated

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

実験手順: N-Chlorosuccinimide (56.1 g) was added slowly to a 0° C. solution of the compound prepared in Example 4 (65.4 g) in N,N-dimethylformamide (1.2 L). The reaction was stirred at room temperature overnight and then diluted with ice water and methyl tert-butyl ether. The layers were separated and the aqueous phase was extracted once more with methyl tert-butyl ether. The organic phases were combined, washed with brine, dried over anhydrous magnesium sulfate and concentrated to obtain the title compound (79.5 g) having the following physical data. The layers were separated the aqueous phase was extracted once more with methyl tert-butyl ether washed with brine dried over anhydrous magnesium sulfate concentrated

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

実験手順: In a similar manner as described in Preparation Example 17, by using methanol (160 mL), 2-chloro-N-hydroxybenzimidoylchloride (8.00 g, 42.10 mmol), methylcyanoacetate (5.22 g, 52.63 mmol) and sodium methoxide (4.55 g, 84.20 mmol), a white solid required compound (9.40 g, 37.21 mmol, 88%) was obtained. In a similar manner as described in Preparation Example 17

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

実験手順: In a similar manner as described in Preparation Example 17, by using methanol (160 mL), 2-chloro-N-hydroxybenzimidoylchloride (8.0 g, 42.10 mmol), methylacetoacetate (9.78 g, 84.20 mmol) and sodium methoxide (6.83 g, 126.30 mmol), a white solid required compound (6.32 g, 25.11 mmol, 60%) was obtained. In a similar manner as described in Preparation Example 17