HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 2-Cyclohexylthiazole-4-carboxylic acid (6-acetyl-3-methoxy-2-methylphenyl)amide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 2-Cyclohexyl-1,3-thiazole-4-carboxylic acid | HCID 23404934 | — |
| Reactant | 2'-Amino-3'-methyl-4'-methoxyacetophenone | HCID 25067316 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 2-Cyclohexylthiazole-4-carboxylic acid (6-acetyl-3-methoxy-2-methylphenyl)amide | HCID 57956452 | 98.3% |
Reaction Steps
POCl3 (1.4 mL, 14.9 mmol) was added drop wise at −35° C. over 5 min, to a stirred solution of 2-cyclohexylthiazole-4-carboxylic acid (117, 1.5 g, 7.1 mmol) and 2-acetyl-5-methoxy-6-methylaniline (1.27 g, 7.1 mmol) in dry pyridine (40 mL). After 1 h, the reaction mixture was successively warmed up to room temperature for 2.5 h, evaporated and neutralized with an aqueous solution of sodium bicarbonate. The precipitate was filtered, washed with water and dried to give 2.6 g (95%) of the title compound 118: m/z=373 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08754106B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-26a3de20715a48c6a42dfa99a7177f6a |
| Source note | uspto-grants-2014_06 |