A kind of synthetic technique of benzyl ribonolactone
A technology of ribolactone and synthesis process, applied in the direction of organic chemistry, etc., can solve the problems of difficult solidification state, not easy to crystallize, and the reaction kettle is locked, and achieves the effect of reducing synthesis cost, shortening process time and reducing loss.
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Embodiment 1
[0033] Embodiment 1: a kind of synthetic technique of benzylribonolactone, comprises the following steps:
[0034] Step 1, the synthesis of compound A2: add 1 equivalent of compound A1 and anhydrous methanol to the reaction kettle, the weight of anhydrous methanol is twice that of compound A1, drop 0.01 equivalent of an acid catalyst at 10°C, the acid catalyst It is methanesulfonic acid, keep it warm at 10°C for 2 hours, after the reaction is monitored by TLC, quench, cool down to 0°C, add 0.01 equivalent of the first pH regulator into the reaction kettle, the first pH regulator is sodium methylate , stirred, concentrated under reduced pressure until no liquid flowed out, then added 1 equivalent of tetrahydrofuran and concentrated until no liquid flowed out, and the obtained light yellow oil was compound A2;
[0035] Step 2, the synthesis of compound A3: add 1 equivalent of compound A2, dimethyl sulfoxide, 4 equivalents of benzyl chloride, 0.2 equivalents of tetrabutylammonium...
Embodiment 2
[0039] Embodiment 2: a kind of synthetic technique of benzylribonolactone, differs from embodiment 1 in that, comprises the following steps:
[0040] Step 1, the synthesis of compound A2: add 1 equivalent of compound A1 and anhydrous methanol to the reaction kettle, the weight of anhydrous methanol is 6 times that of compound A1, and add 0.1 equivalent of acid catalyst dropwise at 13°C, the acid catalyst It is methanesulfonic acid, keep it warm at 13°C for 3 hours, after the reaction is monitored by TLC, quench, cool down to 5°C, add 0.1 equivalent of the first pH regulator to the reaction kettle, the first pH regulator is sodium methoxide , stirred, concentrated under reduced pressure until no liquid flowed out, then added 1 equivalent of tetrahydrofuran and concentrated until no liquid flowed out, and the obtained light yellow oil was compound A2;
[0041] Step 2, the synthesis of compound A3: add 1 equivalent of compound A2, dimethyl sulfoxide, 3.5 equivalents of benzyl chl...
Embodiment 3
[0044] Embodiment 3: a kind of synthetic technique of benzylribonolactone, differs from embodiment 1 in that, comprises the following steps:
[0045] Step 1, the synthesis of compound A2: add 1 equivalent of compound A1 and anhydrous methanol to the reaction kettle, the weight of anhydrous methanol is 10 times that of compound A1, and add 0.2 equivalent of an acid catalyst dropwise at 15°C, the acid catalyst It is methanesulfonic acid, keep it warm at 15°C for 4 hours, after the reaction is monitored by TLC, quench, cool down to 10°C, add 0.2 equivalent of the first pH regulator to the reaction kettle, the first pH regulator is sodium methoxide , stirred, concentrated under reduced pressure until no liquid flowed out, then added 1 equivalent of tetrahydrofuran and concentrated until no liquid flowed out, and the obtained light yellow oil was compound A2;
[0046] Step 2, the synthesis of compound A3: add 1 equivalent of compound A2, dimethyl sulfoxide, 3 equivalents of benzyl ...
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