2-(6-aminopurin-9-yl)-5-(hydroxymethyl)oxolane-3,4-diol: dibutyltin synthesis

Yield:-

Reaction Conditions:

in methanol; for 3 h;Reflux;Time;

Steps:

2.1 (1) by adenosine (I) synthesis of the 2 [...] -O-P-toluene sulphonyl adenosine (III)

Weighing adenosinergic 2.67g, di-n-butyl tin oxide 2.99g, methanol 50 ml, the above-mentioned raw material in a 100 ml round-bottom flask, heating reflow 3h, rotary evaporated to remove methanol after the reaction, generation of the 2 [...], the 3-di-n-butyl armor tin Asia[...] alkyl adenosine (II) directly for the next step reaction, the reaction mixture is added to the toluene sulfonyl chloride 3.10g, triethylamine 2 ml, dichloromethane 50 ml, stir at room temperature reaction 5-7h, concentrating spin vaporization after the reaction, by adding 15 ml methanol, room temperature static 1h, filtered, the filter residue is washed with methanol, then filter residue in the vacuum drying in drying, final obtaining white powdery solid the 2 [...] -O-P-toluene sulphonyl adenosinergic 3.76g, yield 89.2%. HPLC purity of 98.6%.

References:

CN105884846,2016,A Location in patent:Paragraph 0077; 0078; 0079