HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 67121030, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 67121027 | HCID 67121027 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67121030 | HCID 67121030 | 104.2% |
Reaction Steps
Step 2 The intermediate 59 (22.0 mg) was treated with trifluoroacetic acid (327 mg, 2.87 mmol) in anhydrous dichloromethane (0.12 ml). The reaction mixture was stirred at room temperature for 15 minutes, until disappearance of the starting material (HPLC-MS analysis). After that, the reaction mixture was treated with diethyl ether (20 ml) and the residue thus obtained was rinsed with diethyl ether (2×10 ml): the product N-[6-(2,5-dioxo-2,5-dihydro-1H-pyrrol-1-yl)hexanoyl]-L-valyl-N5-carbamoyl-N-(4-{[(piperazin-1-ylcarbonyl)oxy]methyl}phenyl)-L-ornithinamide 60 (white wax, 20.0 mg) was thus isolated and used without further purification in the next step. MS (ESI): 685 [M+H]+. Retention time=2.97 min (method 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08900589B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-2d2f0e73bf4a48118680b397826f2c2c |
| Source note | uspto-grants-2014_12 |