HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 3-[4-(7-chloro-2-methyl-5H-pyrrolo[2,1-c][1,4]benzodiazepin-11-yl)piperazin-1-yl]-2,2-dimethylpropanoic acid di-methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 1-Piperazinepropanoic acid, 4-(7-chloro-2-methyl-5H-pyrrolo[2,1-c][1,4]benzodiazepin-11-yl)-alpha,alpha-dimethyl- | HCID 60148564 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 3-[4-(7-chloro-2-methyl-5H-pyrrolo[2,1-c][1,4]benzodiazepin-11-yl)piperazin-1-yl]-2,2-dimethylpropanoic acid di-methanesulfonate | HCID 86668849 | 96.9% |
Reaction Steps
Add acetonitrile (5 mL) to 3-[4-(7-chloro-2-methyl-5H-pyrrolo[2,1-c][1,4]benzodiazepine-11-yl)piperazin-1-yl]-2,2-dimethylpropanoic acid (0.106 g, 0.255 mmol) to create a slurry. Add methanesulfonic acid (0.050 ml, 0.075 g, 0.76 mmol) to the stirring slurry (1000 rpm) and stir the resultant solution at 60° C. until a white solid precipitates. Cool this slurry, and isolate the solid by filtration to obtain 3-[4-(7-chloro-2-methyl-5H-pyrrolo[2,1-c][1,4]benzodiazepin-11-yl)piperazin-1-yl]-2,2-dimethylpropanoic acid di-methanesulfonate (0.15 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08314092B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-0482f4b9d6b147dcb4b460099dc6ba92 |
| Source note | uspto-grants-2012_11 |