HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 86686956, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 2-{4-[(Tert-butoxy)carbonyl]piperazin-1-yl}acetic acid | HCID 2735642 | — |
| Reactant | 5-Fluoro-2-hydrazinylpyridine | HCID 19916786 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86686956 | HCID 86686956 | 80% |
Reaction Steps
EDC (543 mg, 2.83 mmol) was added portionwise to a solution of 2-(4-Boc-1-piperazinyl)acetic acid (576 mg, 2.36 mmol), 5-fluoro-2-hydrazinyl-pyridine (for reference procedure see WO 2010/022076, which is incorporated herein by reference in its entirety; 0.30 g, 2.36 mmol) and HOBt (32 mg, 0.24 mmol) in dry DCM (15 mL) at RT and stirred for 16 h. The solution was diluted with DCM (20 mL), washed with water (2×20 mL) and dried (Na2SO4). The solvent was evaporated to give the title compound as an off-white solid (667 mg, 80%). LCMS (Method 1): Rt 1.99 min, m/z 354 [MH+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09145413B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-d10d6e06852c47fda0fdeb70fceedd06 |
| Source note | uspto-grants-2015_09 |