HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl chloroformate → Methyl 3-cyano-4-hydroxybenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Methyl 4-hydroxy-3-iodobenzoate | HCID 11346465 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Methyl 3-cyano-4-hydroxybenzoate | HCID 11769089 | 100% |
Reaction Steps
To a stirred solution of 2 (0.376 mol), DIEA (196 mL, 1.13 mol) and THF (200 mL) was added benzyl chloroformate (59.0 mL, 0.414 mol) dropwise. After the reaction solution was stirred at room temperature for 1 hr, the solution was concentrated on a rotovap. The residue was partitioned between sat. NaHCO3 (300 mL) and dichloromethane and the aqueous phase extracted with additional dichloromethane (100 mL×3). The combined dichloromethane layers were dried over sodium sulfate, filtered, and concentrated in vacuo to give product 3 (0.376 mol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07582668B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-cb78595dc0544dadbe24b818ee767e77 |
| Source note | uspto-grants-2009_09 |