HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thioacetamide → Ethyl 2-methyl-4,5,6,7-tetrahydrobenzo[d]thiazole-6-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thioacetamide | HCID 2723949 | — |
| Reactant | Ethyl 3-bromo-4-oxocyclohexane-1-carboxylate | HCID 12917737 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Ethyl 2-methyl-4,5,6,7-tetrahydrobenzo[d]thiazole-6-carboxylate | HCID 12917745 | — |
Reaction Steps
A mixture of EXAMPLE 387A (4.4 g) and ethanethioamide (1.33 g) in N,N-dimethylformamide (50 mL) was heated at 140° C. for 20 hours. After it cooled to room temperature, the reaction mixture was partitioned between water and ethyl acetate. The aqueous layer was extracted with additional ethyl acetate three times. The combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09034875B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-51e7389e38114bae8bc1cf25a7bf8639 |
| Source note | uspto-grants-2015_05 |