With aluminum (III) chloride; sodium hydroxide In toluene at 110℃; Concentration;
Experimental Procedure
the electric stirrer, reflux condenser and a thermometer in four of the reaction bottle, adding m-phthaloyl chloride 20.3g, 2, 2, 6, 6-tetramethyl-4-PIPERIDYLAMINES 36g, solvent 60g, catalyst 1.5g, a reflux condensing tube, thermometer, the agitator is started, the temperature is increased to 110 °C time, start timing, the reaction time is 4.5-10h, after the reaction, under strong stirring, slowly into the reactant in aqueous solution of alkali, to remove the unreacted m-phthaloyl chloride, then return water, lowering the temperature to 15-20 °C to crystallization, filtration can get light stabilizer N, N, -bis-(2, 2, 6, 6-tetramethyl-4-piperidinyl) isophthalamide, light stabilizer N, N, -bis-(2, 2, 6, 6-tetramethyl-4-piperidinyl) isophthalamide the yield reaches 97.38percent, melting point is 270-275°C. | 97.38% |
With sodium hydroxide In water; isopropyl alcohol at 30 – 130℃; under 1125.11 – 2475.25 Torr; Alkaline aqueous solution;
Experimental Procedure
In a 4-necked 2 I flask with stirrer, dropping funnel, thermometer and pH electrode 150.5 [G] of 2,2, 6, 6-Tetramethylpiperidin-4-yl-amine (98.7 percent; 0.95 mole) and 85.2 [G] of 50percent [NAOH] solution (1.07 mole) are added to a mixture of 470.0 [G] of isopropanol and 260.0 g of demin. water. Under stirring 102.1 [G] of molten isophthalic acid chloride (99.4 percent; 0.50 mole) are added. The temperature of the reaction mixture is held at [30°C] during dosage of IPC by cooling with an ice bath. The reaction mixture is stirred for another 1 hour under the same conditions (temperature/pH-control). A white suspension is being formed during this reaction phase. The reaction mixture is transferred to a 3 l laboratory autoclave with stirrer and internal thermometer and the mixture is heated to a temperature of [TI] [100°C.] The resulting pressure of the system is about 1.5 bar and the solid is being dissolved completely. Two liquid phases are being formed: – Lower aqueous phase containing salts and aqueous [NAOH] and some isopropanole – Upper organic phase containing desired product solved in isopropanole ; The lower phase is removed under pressure and 950.0 [G] of demin. water is added to the reaction mixture. The mixture is further heated up to TI = [130° C] and a corresponding system pressure of about PI = 3.3 bar until all of the solid has completely dissolved. The suspension is allowed to cool down to ambient temperature TI [ 30°C.] The resulting white suspension is passed through a filter aggregate with metal screen and the reaction product is washed with 715.0 [G] of demin. water to remove chloride and other impurities. The reaction product is heated in a vacuum drying oven until constancy of weight. The yield of reaction product of general formula [(I)] with Ri = methyl, and R2 = H is 200.0 g or 95.3 percent of theoretical value (yield based on minor component TAD). | 95.3% |
