HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl chloroformate → HCID 19705542, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Pyrazolidinone hydrochloride | HCID 2733712 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19705542 | HCID 19705542 | — |
Reaction Steps
To a suspension of pyrazolidin-3-one hydrogen chloride (5.00 g, 40.8 mmol) in DCM (120 mL) at 0° C. was added DIEA (2.5 eq), followed by CbzCl (1.15 eq). The resulting clear solution was warmed to it and stirred 3 h. The reaction mixture was washed with brine. The aqueous layer was separated and back-extracted with DCM (×2). The combined organic layers were dried over Na2SO4, and concentrated. The crude product was purified by a SiO2 column (0-100% EtOAc/Hexanes, Rf=0.35 in 100% EtOAc) to afford the desired product as a white solid (5.31 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09227971B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-327503e20daf4709984027d54ea6de4e |
| Source note | uspto-grants-2016_01 |