HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 67246087, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Ethyl isocyanatoacetate | HCID 76283 | — |
| Reactant | HCID 67246243 | HCID 67246243 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67246087 | HCID 67246087 | 96.8% |
Reaction Steps
To a solution of Intermediate 58 (3.9 g, 10.7 mmol) in methylene chloride (35 mL) was added ethyl isocyanatoacetate (1.38 mL, 12.3 mmol). The mixture was stirred at room temperature for 5 hours. The crude reaction was cooled to 0° C. and then methanol (2.3 mL) was added. The mixture was stirred at room temperature for 0.5 hours and the solvent was removed under reduced pressure. Purification by column cromatography using methylene chloride/methanol (from pure methylene chloride to 98:2) as eluent gave the title compound (5.1 g, 95%) as oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08420669B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-1ef550d2c3e647beb1defae350f61bad |
| Source note | uspto-grants-2013_04 |