HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloro-4,6-diphenyl-1,3,5-triazine → 2,4-Diphenyl-1,3,5-triazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloro-4,6-diphenyl-1,3,5-triazine | HCID 19698 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2,4-Diphenyl-1,3,5-triazine | HCID 15912 | — |
Reaction Steps
25 g (62.5 mmol) of product b) are dissolved in 200 ml of dimethylformamide under a protective-gas atmosphere, and 7.7 g of 60% NaH in mineral oil (194 mmol) are added. After 1 h at room temperature, a solution of 2-chloro-4,6-diphenyl-1,3,5-triazine (25 g, 68 mmol) in 300 ml of dimethylformamide is added dropwise. The reaction mixture is stirred at room temperature for 12 h. After this time, the reaction mixture is poured onto ice and extracted three times with dichloromethane. The combined organic phases are dried over Na2SO4 and evaporated. The residue is extracted with hot toluene, recrystallised from dichloromethane/isopropanol and finally sublimed in a high vacuum, the purity is 99.9%. The yield is 17 g (27 mmol, 44%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09126970B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-9fc419fa673a47d4a1cec402a14e58cd |
| Source note | uspto-grants-2015_09 |