A kind of 2-phenylbenzothiazole ring metal cobalt catalyst and its synthesis method
A synthesis method and technology of thiazole ring, applied in the field of 2-phenylbenzothiazole ring metal cobalt catalyst and its synthesis, can solve the problems of high production equipment requirements, severe reaction conditions, low process conversion rate, etc., and achieve high conversion efficiency , simple synthesis steps and simple production process
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[0017] A method for synthesizing 2-phenylbenzothiazole ring metal cobalt catalyst, the specific steps are as follows:
[0018] (1) At 0-30℃, diphenylbenzothiazole is used as the starting material, dissolved in an alcohol solvent to make a 0.1-50mol / L solution, and 0.3-0.8 times the mole of the raw material is added. Cobalt chloride hydrate, heated to 80-140°C and stirred for 4-24 hours. After the reaction, it was cooled to room temperature, and the same volume of water as the solvent was added to precipitate the yellow solid product. The yellow solid precipitate was filtered and washed. The intermediate dimer cobalt compound is obtained with a yield of 85%-95%. The dimer is directly put into the next reaction without further purification;
[0019] (2) At 0-30°C, the dimer cobalt compound of the reaction intermediate in the previous step is used as a raw material, dissolved in acetonitrile solvent to prepare a 0.05-5.0mol / L solution, and silver oxide and ammonium hexafluorophosphate...
Embodiment 1
[0030] Add 19.5g 2-phenylbenzothiazole and 6.5g CoCl to a 500mL three-necked flask with a mechanical stirrer and thermometer 2 ·6H 2 O and 250 mL of ethylene glycol were stirred for 10 min, and then the temperature of the reaction system was slowly raised to 120° C., and the reaction was continued for 24 h in contact with the air at this temperature. After the reaction, the reaction solution was cooled to room temperature, cold water was added and the solution was stirred. A yellow solid was slowly precipitated. After standing for 5 hours, it was filtered and the precipitate was washed with ice water. After the precipitate was dried in vacuum, 21.9g of yellow solid was obtained, which is the middle The cobalt compound is a dimer, and the yield is 91%.
Embodiment 2
[0032] Add 19.3 g of the above dimer cobalt compound, 4.65 g of silver oxide and 13.0 g of ammonium hexafluorophosphate into a 500 mL single-necked flask equipped with a stirrer and a thermometer, then add 160 mL of acetonitrile solution, stir for 10 min to form a suspension, and then The reaction system was raised to 60°C and reacted for 16 hours. After the reaction, it was cooled to room temperature. The reaction solution was filtered with Celite and the filter residue was washed with acetonitrile. The mother liquor was subjected to reduced pressure to remove acetonitrile, and the remaining solid was recrystallized with dichloromethane solvent and dried. The yield of 23.7 g of yellow crystals was 88%.
[0033] Product structure identification:
[0034] IR: (film): ν(cm -1 ) 2958, 2904, 2869, 1622, 1589, 1528, 1478, 1445, 1374, 1273, 1224, 1092, 1031, 930, 813, 782, 732, 698.
[0035] 1 H NMR (300MHz, CD 3 CN)δ8.15-7.93(m,4H,Ar-H),7.88-7.80(m,2H,Ar-H),7.72-7.66(m,4H,Ar-H),7.14(t,J=...
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