HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetamidine monohydrochloride → HCID 178439778, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetamidine monohydrochloride | HCID 67170 | — |
| Reactant | Dimethyl propargylmalonate | HCID 4620160 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178439778 | HCID 178439778 | 37% |
Reaction Steps
To a 250 mL flask was added 1 (3.96 g, 20 mmol), 2 (1.85 g, 20 mmol) and 50 mL anhydrous MeOH. After 800 mg (20 mmol) Na was added to the solution, yellow precipitate was observed. The resulting mixture was refluxed overnight. The yellow precipitate was collected by filtration and then dissolved in 10 mL H2O. The pH of the resulting solution was adjusted to 6.5 by adding 2 N HCl to afford a yellow precipitate, which was collected by filtration and dried over P2O5 to afford 1.21 g (37%) of 3: TLC Rf0.11 (CHCl3/MeOH 6:1); mp>300° C.; 1H NMR (DMSO-d6) δ 2.23 (s, 3 H), 3.05 (s, 2 H), 3.32 (s, 1 H), 11.92 (s, 2 H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946239B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-4f3a6081e57d44fd8ceaeda9e7adda5d |
| Source note | uspto-grants-2015_02 |