In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 4131-74-2 as follows. HPLC of Formula: C8H14O4S
Methanol (360 kg) was added to a glass lining kettle, stirred and cooled. The kettle was cooled to 0-5C. Methylamine (180 kg) was introduced within a period of 3-4 hours. After the introduction, the mixture was stirred for 10 minutes while keeping warm. The resultant product was discharged and sealed for storage.; The compound of formula II prepared according to Example 2 and a reacting mother liquid comprising methylamine (35%) were continuously added to the reaction kettle K1 (50 L) from the bottom at a speed of 1 kg per minute and 3 kg per minute, respectively. The resultant product was cooled to the temperature of 0-8C with stirring. The reaction solution overflowing the upper part (5/6 of the total height) of the reaction kettle K1 flowed into the reaction kettle K2 (50 L) from the bottom. The resultant mixture was cooled to the temperature of 0-8C with stirring. The reaction solution overflowing the upper part (5/6 of the total height) of the reaction kettle K2 flowed into the kettles K3 and K4 in the same manner. The reaction solution overflowing the upper part (5/6 of the total height) of the reaction kettle K4 alternately flowed into the centrifuges N1 and N2 having a diameter of 300 mm at a flowing speed of 4 kg/minute for a solid-liquid separation. The mother liquid entered the reaction kettle P (50 L) (in which liquid methylamine was continuously added to the kettle from the bottom at a speed of 0.26 kg/minute). The resultant product was subsequently pumped into the reaction kettle K1. The solid entered the reaction kettles Q1 and Q2 (50 L). The resultant mixture was washed with approximately equal mass of methanol and was subjected to a solid-liquid separation via the centrifuges R1 and R2 (300 mm), respectively. The solid was dried and entered the storage tank T. The experiment was carried out for 20 hours to give 498 kg of the compound of formula V (98.5% via chromatography analysis).
According to the analysis of related databases, 4131-74-2, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Beijing Tianqing Chemicals Co., Ltd.; EP2216331; (2010); A1;,
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