HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → 4-(Chloromethyl)-2-(4-chlorophenyl)-5-ethyl-1,3-oxazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 2-(4-Chlorophenyl)-5-ethyl-4-methyl-1,3-oxazole 3-oxide | HCID 58284303 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 4-(Chloromethyl)-2-(4-chlorophenyl)-5-ethyl-1,3-oxazole | HCID 58284373 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
1.00 g (4.21 mmol) of the compound from example 36A is dissolved in 15 ml of chloroform, and 1.4 ml (15.15 mmol) of phosphoryl chloride is added carefully. The mixture is heated at reflux and stirred at this temperature for 30 min. The mixture is then cooled to 0° C. and made weakly basic using aqueous ammonia. The reaction mixture is extracted three times with in each case 20 ml of ethyl acetate. The combined organic phases are washed once with 10 ml of water and then dried over magnesium sulphate. The solvent is removed on a rotary evaporator, and the residue is dried under reduced pressure in a drying cabinet. Without further purification, the product obtained in this manner is used for the subsequent reactions.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653109B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-81a89afe76e346f2ac1200d3bfb8922e |
| Source note | uspto-grants-2014_02 |