HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 57550254, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 57550255 | HCID 57550255 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57550254 | HCID 57550254 | 70.5% |
Reaction Steps
Acetyl chloride (0.51 ml, 0.72 mmol, 1.2 eq) is added to a cooled (ice bath) solution of (5S)-5-(aminomethyl)-1-{4-[3-(2-methylpyrrolidin-1-yl)propoxy]phenyl}pyrrolidin-2-one 113 (0.2 g, 0.6 mmol, 1 eq) in dichloromethane (12 ml). The mixture is stirred 2 hours at room temperature, washed with a saturated solution of sodium bicarbonate and with brine, dried over magnesium sulfate and concentrated under vacuum to give 0.158 g of yellow oil. The crude material is purified by two chromatographies over silicagel (first one: gradient dichloromethane/methanol/ammonia 100:0:0 to 88:12:1.2; second one: dichloromethane/methanol/ammonia 80:20:2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07943605B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-08130acae2924b3da167fcf645cb7b8b |
| Source note | uspto-grants-2011_05 |