2'-chlorothymidine synthesis
- Product Name:2'-chlorothymidine
- CAS Number:54898-34-9
- Molecular formula:C10H13ClN2O5
- Molecular Weight:276.67
22423-26-3
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Yield:54898-34-9 96.9%
Reaction Conditions:
with hydrogenchloride in N,N-dimethyl acetamide at 60; for 5 h;
Steps:
5 Preparation of 2'-chlorothymidine
The reaction flask was charged with 6% hydrogen chloride in DMA (276.0 g, 0.45 mo 1), 2,2'-anhydro-5-methyluridine(88.0 g, 0.37 mo 1) and heated to 60 ° C for 2 hours. Additional 6% hydrogen chloride in DMA (64.0 g, 0.1 lmo 1) was added and the reaction was continued for 3 hours. The reaction was complete by TLC. The reaction mixture was distilled off under reduced pressure. The residue was added with 70 mL of water and beaten for 1 hour at 50 ° C. The mixture was cooled to room temperature, filtered and the solid was collected. The solid was dried under vacuum at 50 ° C to give 98.2 g The rate of 96.9%, HPLC purity of 99%.
References:
CN103450302,2016,B Location in patent:Paragraph 0111-0113
1463-10-1
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