HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 118023539, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 80400357 | HCID 80400357 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 118023539 | HCID 118023539 | — |
Reaction Steps
To a mixture of 2-amino-5-cyclohexylthiophene-3-carboxamide (53.5 g) and THF (500 mL) were added dropwise acetyl chloride (18 mL) and TEA (36 mL) under ice-cooling, followed by stirring at room temperature for 17 hours. The reaction mixture was concentrated under reduced pressure. To the residue were added EtOH (500 mL) and a 1 M aqueous NaOH solution (500 mL), followed by stirring at 80° C. for 24 hours. The reaction mixture was left to be cooled to room temperature, and 1 M hydrochloric acid (500 mL) was added thereto, followed by stirring. The precipitate was collected by filtration, washed with water, and dried by blowing air to obtain 6-cyclohexyl-2-methylthieno[2,3-d]pyrimidin-4(3H)-one (57.0 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051339B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-decf9bc76a2c4e28b7d05e2508efac06 |
| Source note | uspto-grants-2015_06 |