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With sulfuric acid In dichloromethane; water at 35 - 40℃; for 4.5 h;
To a 500 mL four-necked flask was added 150 mL of dichloromethane,2-carboxy-4'-(N-ethyl-N-isopentyl) -2'-hydroxybenzophenone53.3 g (0.15 mol) and2-methyl-4-methoxydiphenylamine (32 g, 0.15 mol) was added dropwise with stirring40mL 98percent sulfuric acid, to the material all dissolved, the temperature maintained at 35 below. After the dropwise addition, the temperature was raised to 40 ° C4.5h.2). After the reaction was continued, stirring was continued, 150 ml of water was slowly added to the four-necked flask, and the dichloromethane was recovered by heat dissipation,The temperature of the reaction solution was controlled at 65-70 ° C to recover dichloromethane and incubated for 30 min. Add toluene 150mL, continue to heat up toAfter stirring at 85-90 ° C for 30 min, the mixture was stirred, allowed to stand, and the lower acidic aqueous solution was separated. The upper organic phase was added with a small amount of hot waterThe water is about 60 ° C, about 50 g), the organic phase is cooled to below 20 ° C to crystallize, filtered, and the filter cake is treated with a small amount (about 30 ml)Methanol, and dried at 70 ° C for 2 h to give 73.2 g of a white solid, yield 94.2percent. The product was detected by HPLCThe content of the compound was> 99.5percent and the melting point was 166.1-167.8 ° C.In the benzophenone derivative described in this embodiment, R1 represents an ethyl group and R2 represents an isopentyl group. That is, the benzophenone derivative is2-carboxy-4 '- (N-ethyl-N-isopentyl) -2'-hydroxybenzophenone;3- (N-ethyl-N-isopentyl) amino-6-methyl-7-phenylaminofluoran
Reference：
[1] Patent: CN105838105, 2016, A, . Location in patent: Paragraph 0083; 0084; 0085; 0086
With sulfuric acid; In dichloromethane; water; at 35 - 40℃; for 4.5h;
To a 500 mL four-necked flask was added 150 mL of dichloromethane,2-carboxy-4'-(N-ethyl-N-isopentyl) -2'-hydroxybenzophenone53.3 g (0.15 mol) and2-methyl-4-methoxydiphenylamine (32 g, 0.15 mol) was added dropwise with stirring40mL 98percent sulfuric acid, to the material all dissolved, the temperature maintained at 35 below. After the dropwise addition, the temperature was raised to 40 ° C4.5h.2). After the reaction was continued, stirring was continued, 150 ml of water was slowly added to the four-necked flask, and the dichloromethane was recovered by heat dissipation,The temperature of the reaction solution was controlled at 65-70 ° C to recover dichloromethane and incubated for 30 min. Add toluene 150mL, continue to heat up toAfter stirring at 85-90 ° C for 30 min, the mixture was stirred, allowed to stand, and the lower acidic aqueous solution was separated. The upper organic phase was added with a small amount of hot waterThe water is about 60 ° C, about 50 g), the organic phase is cooled to below 20 ° C to crystallize, filtered, and the filter cake is treated with a small amount (about 30 ml)Methanol, and dried at 70 ° C for 2 h to give 73.2 g of a white solid, yield 94.2percent. The product was detected by HPLCThe content of the compound was> 99.5percent and the melting point was 166.1-167.8 ° C.In the benzophenone derivative described in this embodiment, R1 represents an ethyl group and R2 represents an isopentyl group. That is, the benzophenone derivative is2-carboxy-4 '- (N-ethyl-N-isopentyl) -2'-hydroxybenzophenone;3- (N-ethyl-N-isopentyl) amino-6-methyl-7-phenylaminofluoran
With hydrogenchloride; In dichloromethane; water; at 20℃; for 2.0h;
Into a round-bottom flask equipped with a stirring apparatus, 2.59 g (5.0 mmol) of 2?-anilino-6?-(N-ethyl-N- isopentylamino)-3?-methylspiro[phthalide-3,9?-xanthene](Compound 93: trade name, S-205; produced by Fukui Yamada Chemical Co., Ltd.), 1.04 g (10.0 mmol) of concentrated hydrochloric acid (produced by Wako Pure Chemical Industries, Ltd.), 3.81 g (5.0 mmol) of LiFAI3A (produced by Tosoh Finechem Corp.), and 60 mL of dichloromethane were added, and the reaction was carried out at room temperature for 2 hours. After dilution of the reaction solution with dichloromethane, it was washed with water. The solvent was removed from the reaction solution by concentration under reduced pressure to obtain 5.99 g (yield:100percent) of a black solid carboxylic acid derivative having a tetrakis(pentafluorophenyl)borate (IV) anion as a counter anion (Compound 94).
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