1,2,6,7-DIEPOXYHEPTANE synthesis

Yield:4247-19-2 95.8%

Reaction Conditions:

with 3-chloro-benzenecarboperoxoic acid at 8 - 22; for 15 h;

Steps:

4 A one-pot method for preparing diepoxide includes the following steps:

A one-pot method for preparing diepoxide includes the following steps:S1. Epoxidation reaction: At a low temperature, add 10.67g of 1,6-heptadiene to the reactor, slowly add m-chloroperoxybenzoic acid solution dropwise, control the drop acceleration to keep the system temperature at about 8 , and maintain after the dropwise addition The reaction was carried out at a low temperature for 3 hours, then the temperature was raised to 22° C., the reaction was continued for 12 hours, and the reaction was completed to obtain a crude diepoxyheptane solution, in which the molar ratio of diene to m-chlorobenzoyl chloride was 1:2.7;S2. Separation and purification: 238 g of a 20% mass fraction ammonium sulfite aqueous solution was added to the crude diepoxyheptane solution, the system temperature was kept at 20 ° C., the reduction reaction was performed for 2 h, extraction, and the organic phase was separated by extraction. Add 200g mass fraction of 20% ammonium carbonate solution to the organic phase, maintain the system at 20 , neutralize the reaction for 3h, and extract the organic phase. The organic phase was washed twice with water (200 mL × 2), the organic phase was extracted and separated, dried over anhydrous sodium sulfate, the solid filter residue was filtered off, the filtrate was distilled under reduced pressure, the solvent carbon tetrachloride was recovered, and the product was collected to obtain diepoxyheptane .Among them, the preparation method of m-chloroperoxybenzoic acid solution is as follows:Add 38.4g of sodium hydroxide, 250mL of water, 110g of 30% hydrogen peroxide solution, 2.1g of magnesium sulfate heptahydrate to the reactor, stir to dissolve, then add 250mL of dioxane, control the feed temperature at 15 , in the fierce Under stirring, 52.5 g of m-chlorobenzoyl chloride was added all at once, maintaining the reaction temperature at 25 ° C, and stirring for 15 min. Cool down, add 25% hydrochloric acid solution, control the temperature of the system at 10 , acidify to pH 1, add 500mL of carbon tetrachloride, extract and separate the organic phase, dry with anhydrous magnesium sulfate, filter off the solid filter residue to get meta-chloride Oxybenzoic acid/carbon tetrachloride solution.The molar ratio of chlorobenzoyl chloride, sodium hydroxide and hydrogen peroxide is 1:3.2:3.24.The yield of diepoxyheptane was 95.8% and the purity was 93.3%.

References:

CN110981836,2020,A Location in patent:Paragraph 0101-0108