HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22036346, compound → HCID 22036240, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22036346 | HCID 22036346 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Ether hydrochloride | HCID 10953452 | — |
| Product | HCID 22036240 | HCID 22036240 | 69% |
Reaction Steps
The product obtained in Step 1 above was dissolved in a mixture of EtOAc (18 mL) and ether (9 mL) and 5 M HCl/ether (9 mL) was added. The mixture was stirred at room temperature for 3 h. The precipitated hydrochloride salt was filtered off and washed thoroughly with ether. The hydrochloride was dissolved in EtOAc/MeOH/Et3N (100:40:5) and purified by column chromatography) on silica using NH3-satd. EtOAc/CH3OH (100:15) as eluent. The combined pure fractions were concentrated in vacuo and the resulting oil was dried (˜0.8 torr, room temperature) to give 0.36 g (69%) of the title product. HRMS m/z calcd for C19H26N4O4 (M)+374.1954, found 374.1947.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07071180B2 |
| Source dataset | uspto-grants-2006_07 |
| ORD ID | ord-87f51bec0164419d94ede3554fb73ac6 |
| Source note | uspto-grants-2006_07 |