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7483-59-2

3-(1-Piperazinyl)-1,2-propanediol synthesis

5synthesis methods
-

Yield:7483-59-2 95%

Reaction Conditions:

with hydrogenchloride in methanol;water; pH=8.7; for 2.5 h;Inert atmosphere;pH-value;

Steps:

3 synthesis of N- (2,3- dihydroxypropyl) piperazine

Under a nitrogen atmosphere, the reactor 100 ml, was charged with piperazine 8.6 g (0.1 mol), was added with stirring 35% hydrochloric acid 10.4 g (0.1 mol), the internal temperature and 80 ° C did. There, while maintaining the internal temperature below 80 ° C, was added dropwise over 3-chloro-1,2-propanediol 5.6 g (0.05 mol) for 0.5 hours, further stirred remains the same temperature conditions It was continued for 2 hours. Since the reaction liquid was 4.8 where pH was measured, and added of 25% NaOH aqueous solution 6.4 g, and the pH was adjusted to 8.7. Furthermore, maintaining the internal temperature at 80 ° C, stirring was continued for 2 hours to obtain a reaction solution 30.2g of colorless and transparent. Results The product was analyzed by gas chromatography, 95.0% in yield N-(2,3-dihydroxypropyl) piperazine and the selectivity, N-(2,3-dihydroxypropyl) piperazine 96 .8%, N, N'- bis (2,3-dihydroxypropyl) piperazine is 2.9%, unknown content was 0.3%. Results of Example 7 along with the other examples shown in Table 1.[0064]

References:

JP5838628,2016,B2 Location in patent:Paragraph 0058; 0063

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