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ChemicalBook CAS DataBase List METHYL PICOLINIMIDATE
19547-38-7

METHYL PICOLINIMIDATE synthesis

6synthesis methods
-

Yield:-

Reaction Conditions:

with cerium(IV) oxide;carbon dioxide at 119.84; under 750.075 - 7500.75 Torr; for 24 h;Autoclave;

Steps:

Activity tests
General procedure: All the reactions were carried out in an autoclave reactor withan inner volume of 190 ml. A typical procedure of the reaction of CO2 + methanol with 2-cyanopyridine was as follows: 0.34 g of CeO2 catalyst, 0.64 g of methanol (20 mmol, Wako Pure Chemical Industries, 99.8% min.), and 10.4 g of 2-cyanopyridine (100 mmol,Tokyo Chemical Industry Co., Ltd., 99.0% min.) were put into the autoclave together with a spinner, and then, the reactor was purged and pressurized with CO2 (Shimakyu Co. Ltd., >99.5%). Gas line was closed, and then, the reactor was heated to the reaction temperature. The time when the temperature reached the desired reaction temperature is defined as zero reaction time. The mixture was constantly stirred during the reaction. After the specific reaction time, the reactor was cooled to room temperature and the gas was collected. Ethanol (30 ml, Wako Pure Chemical Industries, 99.5% min.) and 1-hexanol (0.2 ml, Tokyo ChemicalIndustry Co., Ltd., 98.0% min.) were added to the liquid phase asa solvent and an internal standard substance for a quantitativeanalysis, respectively. Products in the liquid and gas phases were analyzed by using a gas chromatograph equipped with FID(Shimadzu GC-2014) and GC-MS (Shimadzu QP-2020) with a CP-Sil5 capillary column (length 50 m, i.d. 0.25 mm, film thickness0.25 μm. For the synthesis of various carbonates from CO2 and the corresponding alcohols, the procedures are the same as the case of the reaction of CO2 + methanol with 2-cyanopyridine. After the reaction time, 30 ml of ethanol or acetone (Wako Pure Chemical Industries,99.5% min.) was added to the liquid phase as a solvent, and 0.2 ml of 1-hexanol or 1-propanol (Wako Pure Chemical Industries,99.5% min.) was added to the liquid phase as an internal standard substance for a quantitative analysis. The products in the liquid and gas phases were analyzed by gas chromatography equippedwith an FID or quadrupole mass spectrometer (GC-MS) using a CP-Sil5 capillary column (length 50 m, i.d. 0.25 mm, film thickness 0.25 μm) or TC-WAX capillary column (length 30 m, i.d. 0.25 mm, film thickness 0.25 μm).

References:

Honda, Masayoshi;Tamura, Masazumi;Nakagawa, Yoshinao;Nakao, Kenji;Suzuki, Kimihito;Tomishige, Keiichi [Journal of Catalysis,2014,vol. 318,p. 95 - 107]

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