Preparation method of o-hydroxybenzonitrile
A technology of o-hydroxybenzonitrile and o-hydroxybenzoyl, which is applied in the field of preparation of o-hydroxybenzonitrile, can solve the problems of difficult complete conversion of raw materials, high energy consumption of water removal process, and increased energy consumption, and achieves Avoid the loss of phosgene, the post-processing method is simple and convenient, and the effect of simplifying the operation
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Embodiment 1
[0021] Embodiment 1, the synthesis of o-hydroxybenzonitrile
[0022] Add 138.5 g (1.0 mol) of o-hydroxybenzoyl to the reaction flask, add 0.028 g of arginine, and 700 g of dichloroethane, raise the temperature to 78 ° C, start to feed phosgene, and feed 108.8 g (1.1 mol) for 3 hours , heat preservation reaction 1h;
[0023] After the reaction was finished, about 350 g of dichloroethane was evaporated, the distillation was stopped, the temperature was cooled in an ice bath, and crystals were precipitated, and the temperature was continued to cool to 0° C., stirred for 1 h, filtered, and dried to obtain 118.5 g, the content was 98.5%, and the yield was 98.0% ( as o-hydroxybenzamide).
Embodiment 2
[0024] Embodiment 2, the synthesis of o-hydroxybenzonitrile
[0025] Add 138.5 g (1.0 mol) of o-hydroxybenzoyl to the reaction flask, add 0.056 g of arginine, and 700 g of dichloroethane, raise the temperature to 75 ° C, start to feed phosgene, and feed 108.8 g (1.1 mol) for 4 hours , heat preservation reaction 1h;
[0026] After the reaction was finished, about 350 g of dichloroethane was evaporated, the distillation was stopped, the temperature was cooled in an ice bath, and crystals were precipitated, and the temperature was continued to cool to 0° C., stirred for 1 h, filtered, and dried to obtain 118.6 g, with a content of 98.5%, and a yield of 98.1% ( as o-hydroxybenzamide).
Embodiment 3
[0027] Embodiment 3, the synthesis of o-hydroxybenzonitrile
[0028] Add 138.5 g (1.0 mol) of o-hydroxybenzoyl to the reaction flask, add 0.028 g of lysine, and 700 g of dichloroethane, raise the temperature to 80°C, start to feed phosgene, and feed 108.8 g (1.1 mol) for 3 hours , heat preservation reaction 1h;
[0029] After the reaction is over, distill about 350g of dichloroethane, stop the distillation, cool down in an ice bath, crystals precipitate out, continue to stir, drop to 0°C, stir for 1h, filter, and dry to obtain 118.8g, content 99.1%, yield 98.8% (calculated as o-hydroxybenzamide).
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