HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chlorobenzoyl chloride → HCID 68509333, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chlorobenzoyl chloride | HCID 8501 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 68511840 | HCID 68511840 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68509333 | HCID 68509333 | 51.9% |
Reaction Steps
To a solution of 1-[1-(4-Chloro-benzoyl)-4-hydroxy-pyrrolidin-3-yl]-piperazin-2-one (50 mg, 0.15 mmol) in CH2Cl2 (1 mL) at 0° C., was added DIPEA (27 uL, 0.154 mmol) and 4-Chloro-benzoyl chloride (20 uL, 0.154 mmol). The mixture was stirred at RT for 4 h. The organic phase was washed with Sat. NaHCO3, dried over Na2SO4, and concentrated. The residue was purified by column chromatography (Ethyl acetate:Methanol:Et3N:10.1:0.1) to give the desired product (36 mg, 50% yield) as a white solid. MS: (ESI), M/Z, 462 (M+1). Retention time: 2.25 min (FA-polar).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07635698B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-0ab2eb897e77401792f20077b3227a4d |
| Source note | uspto-grants-2009_12 |