反应详情

304 mg (1.91 mmol) of 3-amino-2-naphthol, 477 mg (1.81 mmol) of methyl 2-chloro-3,5-dinitrobenzoate and 178 mg (2.17 mmol) of sodium acetate were suspended in a mixture of water (5 ml) with ethanol (10 ml) and heated under reflux for 7 hours. After adding 3 ml of a 2 N aqueous solution of sodium hydroxide thereto, the reaction mixture was heated under reflux for additional 2.5 hours and then brought back to room temperature. After adding 10 ml of 1 N hydrochloric acid thereto, the precipitate thus formed was recovered by filtration and washed successively with water, 1 N hydrochloric acid and ethanol to thereby give 430 mg of 3-nitro-12H-benzo[b]phenoxazine-1-carboxylic acid. Then this product was treated by the same methods as those of Production Example 23 and Example 13 to thereby give the title compound.

1. temperatureheated
2. temperatureunder reflux for 7 hours
3. temperaturethe reaction mixture was heated
4. temperatureunder reflux for additional 2.5 hours
5. custombrought back to room temperature
6. customthe precipitate thus formed
7. filtrationwas recovered by filtration
8. washwashed successively with water, 1 N hydrochloric acid and ethanol