HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aluminum(III) Chloride → 6-(6-chloro-2-methyl-pyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | 4-Methyl-3H-benzooxazol-2-one | HCID 12709336 | — |
| Reactant | 6-Chloro-2-methylpyrimidine-4-carbonyl chloride | HCID 19018481 | — |
| Product | 6-(6-chloro-2-methyl-pyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one | HCID 58181118 | — |
Reaction Steps
2.48 g (13.0 mmol) 6-chloro-2-methyl-pyrimidine-4-carboxylic acid chloride, 1.94 g (13.0 mmol) 4-methyl-3H-benzoxazol-2-one and 6.93 g (52.0 mmol) aluminium trichloride were heated to 125° C. with stirring for 1.5 h. The mixture was combined with ice water and the precipitate formed was suction filtered and washed with water. Then the precipitate was dissolved in MeOH/DCM and suction filtered through silica gel. The filtrate was evaporated down and the residue was purified by flash chromatography. The fractions containing the product were combined, evaporated down and triturated with diethyl ether. The precipitate was suction filtered, washed with diethyl ether and dried i. vac.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450327B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-3842139c505546a98c7bafa55bd5797b |
| Source note | uspto-grants-2013_05 |