Formaldehyde → HCID 178442629, compound

Participants

Reaction Conditions

Reaction Steps

To a container with a stirrer, 63.4 kg of 4-(1,1,3,3-tetramethylbutyl)-6-benzotriazolyl phenol, 5.2 kg of paraformaldehyde, 11.0 kg of diethylamine and 60 L of xylene were charged, and reacted at a temperature of 95 to 100° C. for 24 hours. Then, 3.1 kg of 28% sodium methylate solution in methanol was added and reacted under nitrogen gas at temperature of 145 to 150° C. for 10 hours. The reaction solution was washed with water, and crystallized by cooling the xylene layer to 10° C. The resulting crystal was filtered to obtain 56.8 kg (yield 88%) of 2,2′-methylenebis[4-(1,1,3,3-tetramethylbutyl)-6-benzotriazolylphenol] as white solid in a shape of fine powder (causing dust). Powder X-ray diffraction analysis for the resulting crystal with Cu-Kα radiation indicated that it was type I having distinct diffraction peaks at diffraction angles (2θ±0.1°) of 7.1°, 8.6°, 14.3°, 16.1°, 18.1° and 23.0° as shown in FIG. 4. Further, DSC analysis indicated that the crystal was 100% type I as shown in FIG. 5.

Provenance & Evidence