HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalyl chloride → 5-Thiazolecarboxylic acid, 4-methyl-, ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 4-Methylthiazole-5-carboxylic acid | HCID 209805 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-Thiazolecarboxylic acid, 4-methyl-, ethyl ester | HCID 298610 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
4-methylthiazole-5-carboxylic acid was dissolved in DCM, cooled to 0° C., added oxalyl chloride (7.6 ml, 88 mmol) and DMF (2 drops). Reaction mixture was stirred for 30 mins and DCM was removed on rotavapour. Residue was dissolved in MeOH at 0° C. and stirred for 30 mins at rt. MeOH was removed on rotavapour and crude was worked up (AcOEt/H2O) to obtain the title compound (4.1 g) as a white solid. 1H-NMR (δ ppm, CDCl3, 400 MHz): 8.83 (s, 1H), 4.35 (q, J 7.2, 2H), 2.78 (s, 3H), 1.37 (t, J 7.2, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08377970B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-33fbc738728e46069d2441eefef4fc06 |
| Source note | uspto-grants-2013_02 |