Tricine synthesis
- Product Name:Tricine
- CAS Number:5704-04-1
- Molecular formula:C6H13NO5
- Molecular Weight:179.17
Yield:-
Reaction Conditions:
Stage #1: 2-amino-2-hydroxymethyl-1,3-propanediol;cyanomethyl bromide in acetonitrile at 60; for 4 h;
Stage #2: with water in acetonitrile at 90; under 150.015 Torr; for 6 h;
Steps:
3 Example 3
Preparation method of tris (hydroxymethyl) methylglycine, comprising the following preparation steps: Preparation step S1: Under stirring conditions, 20g of compound I trimethylolomethane, compound A, reaction solvent acetonitrile were added to the drying reactor of 1L, the molar ratio of compound I and compound A was 1:2, the reaction oil bath temperature was 60 °C, the reaction pressure was -0.01MPa (gauge pressure), and the reaction time was 4h. After the completion of the reaction, it is reduced to room temperature, the insoluble substances are filtered out, the filtrate is rotated under reduced pressure and evaporated to remove the solvent, concentrated, and the crude product of Compound II is prepared; Where compound A is Y is Br. Preparation step S2: Under stirring conditions, 20g of compound II, reaction solvent acetonitrile were added to the 1L drying reactor, water was added, hydrolysis reaction occurred with water, the reaction oil bath temperature was 90 °C, the reaction pressure was 0.02MPa (gauge pressure), the reaction time was 6h, and then the acid-base treatment reaction was carried out. After the completion of the reaction, it was reduced to room temperature, the insoluble matter was filtered out, the filtrate was reduced under reduced pressure and rotated to evaporate to remove the solvent, concentrated, and the crude product was prepared to give a crude tris (hydroxymethyl) methylglycine, with a crude product yield of 94%. Preparation step S3: Under dry conditions, using drying and sealing equipment, the crude tris (hydroxymethyl) methylglycine obtained in step S2 was dissolved in purified solvent acetonitrile, and then recrystallized, and then crystallized, filtered and dried under low temperature conditions to obtain a refined tri(hydroxymethyl) methylglycine product with a fine purity of 99.7%.
References:
CN113861053,2021,A Location in patent:Paragraph 0064-0076
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