HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 71812076, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | HCID 86699695 | HCID 86699695 | — |
| Product | HCID 71812076 | HCID 71812076 | 61% |
Reaction Steps
A solution of methyl chloroformate (1.2 mL, 12 mmol) was added drop wised to a stirred solution of compound 2 (1.44 g, 4 mmol) in dry anhydrous tetrahydrofuranipyridine (30 mL) at 0° C. The mixture was refluxed for 3 h. After 10 h stirring at room temperature, the pH value of the mixture was adjusted to pH=6 by 5% HCl(aq). The mixture was cooled to obtain crystalline compound on an ice bath for 2-3 h. After cooling, precipitated crystals were filtered off and washed with diluted HCl and water. The crude product was purified by crystallization from hot ethanol to afford compound 14.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09162993B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-e2432989361e4f269c31368f250b0bdf |
| Source note | uspto-grants-2015_10 |