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ChemicalBook CAS DataBase List Chlorocyclohexane
542-18-7

Chlorocyclohexane synthesis

15synthesis methods
-

Yield:542-18-7 97%

Reaction Conditions:

with hydrogenchloride;tetrabutyl-ammonium chloride;sodium chloride in water at 20; for 5 h;Reagent/catalyst;

Steps:

1 Example 1
S1: Take 7g of sodium chloride and 2.5ml of hydrochloric acid (mass fraction 35%), stir and dissolve in 50ml of water to obtainan aqueous solutioncontaining halide Cl- -wherein hydrochloric acid and sodium chloride are used together as a chlorination agent;S2:An aqueous solutioncontaining a halide Cl-is placed in a photoreactor, and 0.3 g of nanosilver/silver chloride is added to the photoreactor as a photocatalyst (silver nanosilver loading 8.6 mol %) and 0.05 g tetrabutyl chloride. Ammonium as a phase transfer catalyst, and finally added 15ml of cyclohexane;S3: Under strong magnetic stirring, turn on the 300W Xenon lamp and react at room temperature for 5h;S4: After the reaction solution is allowed to stand, the photocatalyst is recovered by filtration, the aqueous phase is separated and recovered, and the organic phase is dried, and the dried organic phase is subjected to rectification and purification to obtain the corresponding organic halogenated product.Sampling was analyzed by GS. The conversion rate was 46% and no polychlorinated product was detected.Distillation collects the 141.5-142.5° C. fraction, ie chlorocyclohexane, with a yield of 97%.As shown in Figure 1, Figure 1 shows the GC-MS of the final reaction mixture.Figure 2 is an HNMR chart of the final major product, chlorocyclohexane.In the present invention, the so-called "loading amount" means that the nano metal accounts for the mole percentage of the nano metal/semiconductor composite material.

References:

Hebei University of Science and Technology;Liu Shouxin;Zhang Qi;Tian Xia;Fan Shiming;Huang Jing CN106831314, 2017, A Location in patent:Paragraph 0031-0037; 0048; 0049

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