Yield:1132-61-2 81%

Reaction Conditions:

in ethanol;water at 0; for 2 h;Large scale;

Steps:

1; 2; 2; 3 Example 1

General procedure: 2500L of pretreated anhydrous ethanol (water content <0.02%) was added to a 5000L glass-lined reactor, and 800 kg of molten 1,3-PS was added under stirring. The mixture was stirred and cooled to 25-30 ° C, and the temperature was controlled for 4 hours.582 kg of morpholine was added dropwise, and the reaction was carried out at this temperature for 2 hours, and dropped to 0 ° C.The crystal was incubated for 10 hours, and 2160 kg of wet product was obtained by centrifugation, and the alcohol obtained by the mother liquor was recovered for recrystallization. Add 1600L of alcohol to the 3000L glass jar, add 300kg of deionized water, add 1080kg of the wet product obtained by the step, stir to 70 ° C, add deionized water to make the wet product completely soluble, add 1kg of insurance powder, 25kg of medicine Using activated carbon, decolorize for 1 hour, press filter, the filtrate enters the crystallization tank, and then add 1600L alcohol to wash the tank. Pass the filter to enter the crystallization tank. Under nitrogen protection, heat up and dissolve. After total dissolution, slowly stir and cool down to 35~40 °C. When it becomes turbid, it will be moisturized and crystallized for 1 hour, then cooled to 0~5 °C, centrifuged, washed twice with 20L of absolute ethanol, dried, placed in a rotary vacuum dryer, controlled temperature below 80 °C, vacuum degree above 0.08MPa , dry to the product qualified, get 548kg of product, yield 80% (in terms of 1,3-PS), sampling test: content 99.8% (alkali titration),The UV absorbance of the 0.5 M aqueous solution at 260 nm and 280 nm was 0.02.

References:

CN109836397,2019,A Location in patent:Paragraph 0023-0027; 0030-0033