Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 178442657 | HCID 178442657 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 178442629 | HCID 178442629 | 157.1% |
Reaction Steps
To a container with a stirrer, 634 g of 4-(1,1,3,3-tetramethylbutyl)-6-benzotriazolyl phenol, 52 g of paraformaldehyde, 110 g of diethylamine and 600 ml of xylene were charged, and reacted at a temperature of 95 to 100° C. for 24 hours. Then, 31 g of 28% sodium methylate solution in methanol was added and reacted at a temperature of 145 to 150° C. for 10 hours. Upon completion of the reaction, the reaction solution was washed with water, 100 ml of methyl isobutyl ketone was added to the xylene layer and crystallized. The resulting crystal was filtered to obtain 594.0 g (yield 92%) of 2,2′-methylenebis[4-(1,1,3,3-tetramethylbutyl)-6-benzotriazolylphenol] as white crystal (causing no dust) with a melting point of 199 to 200° C. The resulting compound had a mass of 659 (calculated value 658.9) in mass spectrometry. In addition, powder X-ray diffraction analysis with Cu-Kα radiation indicated that the resulting crystal was a crystal material 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. 1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07326744B2 |
|---|
| Source dataset | uspto-grants-2008_02 |
|---|
| ORD ID | ord-f3e01d3348084ee3bb2a1782c72db5fd |
|---|
| Source note | uspto-grants-2008_02 |
|---|