166376-97-2Relevant articles and documents
Deoxyribonolactone lesion in DNA: Synthesis of fluorinated analogues
Crey, Caroline,Dumy, Pascal,Lhomme, Jean,Kotera, Mitsuharu
, p. 1093 - 1095 (2003)
Mono- and difluorinated derivatives of 2-deoxyribonolactone were synthesized using diastereoselective Reformatski reaction as a key step.
High-selectivity synthesis method for gemcitabine intermediate
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, (2021/01/29)
The invention discloses a high-selectivity synthesis method for a gemcitabine intermediate. The high-selectivity synthesis method specifically comprises the following process: Step 1, synthesis of T1;Step2, synthesis of T2, to be specific, 550kg of hydrogen peroxide is dropwise added into the T1, and a reaction is controlled to produce the T2; Step3, synthesis of T3, to be specific, sodium acetate trihydrate or sodium carbonate is added into a reaction kettle, the PH value is adjusted with glacial acetic acid, a 10%-15% sodium hypochlorite aqueous solution is dropwise added, and a reaction iscontrolled to produce the T3; Step 4, synthesis of T4; Step 5, synthesis of T5; Step 6, synthesis of T6; Step 7, synthesis of T7; Step 8, synthesis of T8; and Step9, T8 configuration transformation.The high-selectivity synthetic method for the gemcitabine intermediate can reduce the production cost, and meanwhile, can also increase the yield of the gemcitabine intermediate.
Preparation method of intermediate of antitumor drug gemcitabine hydrochloride
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, (2020/10/14)
The invention relates to a preparation method of a intermediate of antitumor drug gemcitabine hydrochloride. According to the method, D-isoascorbic acid is used as a starting raw material and reacts with 2,2-dimethylpropane under the catalysis of p-toluenesulfonic acid in the presence of acetone serving as a solvent to protect hydroxyl groups at 5 and 6 sites to obtain T1; then, hydrogen peroxideis used for carrying out oxidation under the alkaline condition to obtain T2; the T2 is oxidized by sodium hypochlorite to obtain T3; the T3 and ethyl bromodifluoroacetate are subjected to a Reformatsky reaction to obtain T4; then the T4 is subjected to deprotection and cyclization under the catalysis of trifluoroacetic acid to obtain T5; the T5 and benzoyl chloride are subjected to an esterification reaction under the catalysis of DMAP to obtain T6, and a synthetic route II is shown in the specification.