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ChemicalBook CAS DataBase List DL-1,4-DICHLORO-2,3-BUTANEDIOL
7268-35-1

DL-1,4-DICHLORO-2,3-BUTANEDIOL synthesis

5synthesis methods
-

Yield:7268-35-1 67%

Reaction Conditions:

with potassium permanganate in water;acetone; for 5 h;Industrial scale;

Steps:

1 Example 1

In a three-necked flask, 10 g of cis-1,4-dichloro-2-butene (Sinopharm Shanghai Chemical Reagent Company, chemically pure) was dissolved in 60 mL of acetone and 20 mL of water,Into ice water to the system temperature was 0 -5 , 15.16g potassium permanganate (Sinopharm Shanghai Chemical Reagent Company, pure chemical) was added in three batches.The reaction was monitored for 5 hours, the reaction was complete by TLC monitoring, the solid was removed by suction filtration, activated carbon by adding appropriate amount of activated carbon after filtration, the acetone was distilled off under reduced pressure, ethyl acetate was added, washed with saturated sodium chloride solution,The organic phase was separated, dried over anhydrous sodium sulfate and evaporated to dryness. The residue was purified by beating with a 1: 6 volumetric mixture of ethyl acetate and petroleum ether at reflux.8.5 g of 1,4-dichloro-2,3-dibutyl alcohol of the formula (I) was obtained in a yield of 67%.

References:

CN107235872,2017,A Location in patent:Paragraph 0013; 0042; 0043; 0045; 0047; 0049; 0051