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ChemicalBook CAS DataBase List CYASORB UV-3638

CYASORB UV-3638 synthesis

6synthesis methods
-

Yield:18600-59-4 99%

Reaction Conditions:

Stage #1: anthranilic acid;terephthaloyl chloride in N,N-dimethyl acetamide at 0 - 5; for 1 h;Cooling with ice-methanol;
Stage #2: with acetic anhydride in N,N-dimethyl acetamide;toluene; for 1.5 h;Product distribution / selectivity;Heating / reflux;

Steps:

2

Example 2(Preparation of exemplified compound (1-7))120.7 g of anthranilic acid and 1000 ml of N,N-dimethylacetamide were placed in a three-necked flask, and the mixture was dissolved while agitated. 89.3 g of terephthaloyl chloride was added to the mixture while the mixture was stirred continuously; the resulting solution was cooled in an ice-methanol bath; and the mixture was agitated additionally for 1 hour. The internal temperature was 0 to 5°C at the time. Then, 225 g of acetic anhydride and 500 ml of toluene were added thereto; the mixture was heated and agitated under solvent reflux for 1.5 hours and then cooled to 3O0C or lower; and the crystal obtained was filtered and dried, to give 160.5 g of a target exemplified compound (1-7) (yield: 99%). The content of sodium and potassium in the exemplified compound obtained (1-7) was 1 ppm or less. Melting point: 316.3 °C Maximum absorption wavelength (λ max) in solution: 349.5 nm (toluene solution)

References:

WO2009/41715,2009,A1 Location in patent:Page/Page column 18; 19

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