HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl chloroformate → HCID 68576719, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl chloroformate | HCID 6586 | — |
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Reactant | HCID 68584820 | HCID 68584820 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68576719 | HCID 68576719 | — |
Reaction Steps
HCl-dioxane (1 mL, 4.0 M) was added to 78a (Ar1=Ph, Ar2=4,6-dimethyl-pyrimidin-5-yl, 40 mg, 0.073 mmol). The mixture was stirred at RT for 90 min. The solvent was removed, and the residue was dried in vacuo. Methyl chloroformate (8 μL, 0.10 mmol) was added to a solution of the residue from the deprotection, TEA (16 μL, 0.11 mmol) in DCM (0.5 mL) maintained at 0° C. The reaction mixture was stirred and warmed to RT. The crude product was purified on a preparative TLC plate developed with a 45:55 mixture of DCM and DCM/MeOH/NH4OH (60/10/1) to afford 0.004 g (11%) of V-7.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07625905B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-d3a63a15323149fb9d3aca3b00608bf6 |
| Source note | uspto-grants-2009_12 |