HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl chloroformate → HCID 86726387, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 86726386 | HCID 86726386 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86726387 | HCID 86726387 | — |
Reaction Steps
To a stirred solution of the product from step 3 (80 mg, 0.1 mmol) in dichloromethane (2 mL) was added triethylamine (0.02 mL, 0.16 mmol) and methyl chloroformate (0.01 mL, 0.12 mmol). The mixture was stirred at ambient temperature for 6 h, then diluted with dichloromethane (10 mL) and washed with aqueous NaHCO3 and brine. The organic phase was dried (MgSO4), filtered, and the solvents were removed in vacuo. The residue was chromatographed on a 12 g SiO2 column using a gradient elution of 0-100% EtOc in hexanes. Fractions containing product were combined and the solvents were removed in vacuo to give the title compound as a gum. (M+H)+=825.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09315475B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-a8c2be5aff65400f84b5ccdf10bfad1d |
| Source note | uspto-grants-2016_04 |