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ChemicalBook CAS DataBase List TRANS-1,2-CYCLOHEXANEDIOL

TRANS-1,2-CYCLOHEXANEDIOL synthesis

11synthesis methods
-

Yield:-

Reaction Conditions:

with hydrogen in n-heptane at 119.84; under 51005.1 Torr; for 8 h;Kinetics;Autoclave;Inert atmosphere;Solvent;

Steps:

Activity tests

General procedure: Activity tests as well as reduction of catalysts were performed ina 190 ml stainless-steel autoclave with an inserted glass vessel. Thecatalyst (25-100 mg), a spinner and reaction solvent (n-heptaneor water; typically 10 ml) were put into an autoclave and heatedat 473 K under 8 MPa H2(Nippon Peroxide Co., Ltd.) for 1 h forthe reduction pretreatment. After the pretreatment, the autoclavewas cooled and H2was removed. The substrate was quickly putinto the autoclave. After sealing the reactor, the air was purgedby flushing three times with 1 MPa N2(Tanuma Sanso). The auto-clave was heated to the reaction temperature (393 K) under N2.The temperature was monitored by using a thermocouple insertedinto the autoclave. After reaching the reaction temperature, H2wasintroduced to start the reaction. Typical H2partial pressure was6.8 MPa with the total pressure of 8 MPa. Commercial catalysts andRh ReOx/SiO2catalyst were used without reduction pretreatmentsince they can be readily reduced with H2below the reaction tem-perature (393 K). After an appropriate reaction time, the reactorwas cooled in water, and the gases were collected in a gas bag.The products in both gas and liquid phases were analyzed by GC(Shimadzu GC-2014) equipped with an InertCap 5MS/Sil or TC-WAX capillary column and FID. Products were also identified usingGC-MS (QP5050, Shimadzu).

References:

Nakagawa, Yoshinao;Mori, Kazuma;Chen, Kaiyou;Amada, Yasushi;Tamura, Masazumi;Tomishige, Keiichi [Applied Catalysis A: General,2013,vol. 468,p. 418 - 425]

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