HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 69740869, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 1-Boc-Azetidine-3-carboxylic acid | HCID 2755981 | — |
| Reactant | HCID 131725244 | HCID 131725244 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69740869 | HCID 69740869 | 76% |
Reaction Steps
The title compound was prepared according to the procedure described in Example 10 (Step b) using N-((1R)-1-[(4-chlorophenyl)methyl]-2-oxo-2-{4-[2-(2-oxo(4-imidazolinyl))phenyl]-piperidyl)ethyl) (tert-butoxy)carboxamide (Example 18 Step b) (0.227 g, 0.433 mmol) and satd HCl in EtOAc (20 mL), followed by Boc-azetidine-3-carboxylic acid (PepTech Corporation) (0.105 g, 0.52 mmol), EDC (Advanced ChemTech) (0.125 g, 0.65 mmol), HOBT (Novabiochem) (0.058 g, 0.433 mmol) and TEA (Aldrich) (0.058 mL, 0.433 mmol) in CH2Cl2 (10 mL). Purification by silica gel chromatography (100% EtOAc then 1:9 MeOH:EtOAc) provided the title compound as a white foam (0.2 g). MS (ESL pos. ion) m/z: 608 (M+1). Calc'd for C32H38ClN5O5: 607.26.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06977264B2 |
| Source dataset | uspto-grants-2005_12 |
| ORD ID | ord-e4f5fb616c5640da86471414118799a3 |
| Source note | uspto-grants-2005_12 |