Sulfuric Acid → UV-328

関与物質

反応条件

反応手順

Example 1 from U.S. Pat. No. 4,835,284 is duplicated. 2-nitro-2'-hydroxy-3',5'-di-t-amylazobenzene (12.8 g) is added to a mixture of methanol (41 g), water (10 g) and 97% sodium hydroxide (11 g), and the resultant mixture is stirred at 65° C. for 30 minutes. Thereafter, 9-fluorenone (2.0 g) and then glucose (12 g) are added to the mixture at 60° C. to 65° C. over 4 hours. The resultant mixture is further stirred for 4 hours at the boiling point (70° C.), thus completing the reduction reaction. Thereafter, water (50 ml) is added to the reaction liquor, and the reaction liquor is neutralized with 62% sulfuric acid (13 g). The liquor thus neutralized is cooled to 20° C. to precipitate a crystal. The crystal thus obtained is separated by filtration, and the separated crystal is fully washed with water and further with methanol. The washed crystal is then dried, thus producing 9.9 g of 2-(2'-hydroxy-3',5'-di-t-amylphenyl)-benzotriazole having a melting point of 77° to 79° C. at the yield of 85.0%. One can see that reduction using the aromatic ketone 9-fluorenone takes over 81/2 hours.

情報源と証拠