HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Malonate → HCID 178516644, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Malonate | HCID 7761 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | 4-(Trifluoromethyl)thiazole-2-carboximidamide hydrochloride | HCID 66730474 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178516644 | HCID 178516644 | 98% |
Reaction Steps
To a stirred solution of NaOEt (32 g, 5 eq.) in EtOH (200 mL) was slowly added compound 282 (22 g, 1 eq.). The reaction mixture was stirred at room temperature for 30 min and diethyl malonate (11.5 mL, 0.8 eq.) was then added. The suspension was refluxed for 24 hrs. The solvent was removed under reduced pressure. The residue was suspended in H2O (200 mL) and acidified to pH 5 with 2 N aqueous HCl. The resulting solid was filtered, washed with water, and dried under reduced pressure to yield compound 283 as a brown solid in 98% yield. 1H NMR (DMSO-d6, 400 MHz) δ 5.77 (s, 1H), 8.68 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09353100B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-8a3c7c5829324d51a0c5bd235c1aa426 |
| Source note | uspto-grants-2016_05 |