Dinucleotide and synthesis method thereof
A dimeric nucleotide and synthesis method technology, applied in the field of dimeric nucleotide synthesis, can solve problems such as low yield and limited scale production
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Embodiment 1
[0082] raw material:
[0083] Compound 1
[0084] Compound 2
[0085] Raw material treatment: 45.23g (0.9eq) of compound 1 and 34.9g of compound 2 were dehydrated and dried with 350ml of dichloromethane DCM with water.
[0086] In the first step, add the above compound 1 and compound 2 into the flask, and add 4.1 g (1.0 eq) of tetrazole therein. Reacted at 26°C for 14h. Purification: extract with sodium bicarbonate and sodium chloride aqueous solution, dry the organic phase, filter and concentrate; then use 17 times the mass of silica gel chromatography for elution, and the eluent is 10 times the column volume of Hep / EA = 1 / 2. After elution, the eluate containing compound 3 (content 88.09%) was collected, and then the eluate was concentrated to dryness to obtain 40.0 g of solid. The purity of compound 3 was 97.30%.
[0087] Structure of compound 3
[0088] In the second step, 34.5g (1.0ep) of compound 3 was mixed with 345ml of dichloromethane DCM and 7.7mL (1.5eq) ...
Embodiment 2
[0099] Raw material treatment: 31.0 g of compound 1 was added, 39.41 g (0.9 eq) of compound 2 were added and dried with DCM.
[0100] In the first step, compounds 1 and 2 were dissolved in 500ml of DCM, 3.85g (1.0eq) of tetrazole was added, and reacted at 25±2°C for 12h. Then the aqueous solution was extracted, the organic phase was dried, filtered and concentrated, 16 times packed silica gel chromatography, 8 times the column volume Hep / EA=1 / 1.5 elution collected the next column liquid, concentrated under reduced pressure to dryness to obtain 57.0 g of compound 3 product, purity: 83.97% ; The conversion rate of compound 2 was 85.29%.
[0101]
[0102] In the second step, 48.45g (1.0eq) of compound 3 was dissolved in 485ml of DCM, and 11.6ml (1.5eq) of tert-butanol peroxide was added. After reacting at 25±2°C for 1h, TLC monitored that there was no raw material. Use 2.5eq thio Sodium sulfate aqueous solution was quenched, washed twice with water, and 60.0 g of compound 4 (pu...
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