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67-47-0 Synthesis

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Yield:65313-46-4 93.3%

Reaction Conditions:

with formic acid;C₃₄H₅₀Ir₂N₄O₆⁽⁴⁺⁾*2O₄S^(2-);sodium formate at 130; pH=2.5; for 2 h;Reagent/catalyst;Temperature;pH-value;

Steps:

11

Weigh 1mmol5-HMF (126mg), using 1mol / L of formic acid 5mlpH = 2 / dissolving sodium formate buffer solution and transferred to a 35mL glass pressure tube was added 200μL 2 catalyst (catalyst concentration: [Cp * Ir- (di-R -bpy) (OH₂)] SO₄Complexes 0.50mmol / L), i.e. 100ppm (when compared to a dual site catalyst Ir 50ppm) catalyst, with magnetic stirring and the reaction was heated in an oil bath 120 2H; After completion of the reaction, ice-water bath and cool to room temperature.The 5-HMF feedstock quality similar dimethyl phthalate internal standard added to the reaction mixture, washed with methanol and 20ml wall.After the mixed reaction liquid to take appropriate centrifuge tube, with a larger volume of the reaction solution was taken in methanol and then diluted into after centrifugation centrifuge.Gas chromatography (GC (2104, Shimazu, FID) fitted on the DM-WAX (30m × 0.32mm × 0.25μm) for detecting the column combination in gasifier temperature setting 250 , detector temperature setting 280 , column oven temperature setting 180 holding 20min. linear velocity of 45cm / s, split ratio was 50.) reacting a compound of quantitative detection system, measured HHD yield was 36.2%Specific reaction and detecting the same manner as in Example 1, except that the catalyst was changed to the catalyst 8, formic acid / sodium formate buffer solution adjusted to pH 2.5, the reaction temperature was 130 .The resulting product is 1-hydroxy-2,5-dione (the HHD) in a yield of 93.2%

References:

CN105712854,2016,A Location in patent:Paragraph 0074; 0075

67-47-0 Synthesis

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110-13-4 Synthesis