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ChemicalBook CAS DataBase List FLUORESCEIN CHLORIDE
630-88-6

FLUORESCEIN CHLORIDE synthesis

4synthesis methods
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Yield:630-88-6 90.5%

Reaction Conditions:

with sulfolane;thionyl chloride in N,N-dimethyl-formamide at 60 - 80; for 2.5 h;Temperature;

Steps:

1 1, the synthesis of intermediate A, the reaction is as follows:

In the presence of a stirrer,thermometer,Reflux condenser and acid gas absorption device in the three bottles,50 g (0.15 mol) of fluorescein (C20H12O5) was added,1.46 g (0.02 mol) of dimethylformamide (DMF)with200 ml of sulfolane (C4H8O2S),Was added to a 500 ml reactor,Stirring and heating to 60 ° C,70.8 g (0.60 mol) of thionyl chloride (SOCl2) was added dropwise,About 30 minutes dripping finished,Continue to heat up to 80 ° C,Insulation reaction 2h,The reaction ends,Cooling it to about 30 ° C,And then poured into 250ml volume ratio of 1: 1 in the mixture of acetone and water,Stirring and stirring 2h after filtration,Filter cake with 50ml volume ratio of 1:1 mixture of acetone and water leaching,Dried to light yellow intermediate A 50g,The yield was 90.5 wt% and the content was about 96.5 wt%.

References:

CN106967304,2017,A Location in patent:Paragraph 0028; 0029; 0030; 0031; 0032; 0048

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