HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → (S)-2-Butyl-10-(4-methyl-3-phenethyl-piperazin-1-yl)-4H-3-thia-1,4,9-triaza-benzo[f]azulene dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | (S)-2-Butyl-10-(4-methyl-3-phenethyl-piperazin-1-yl)-4H-3-thia-1,4,9-triaza-benzo[f]azulene | HCID 136005597 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | (S)-2-Butyl-10-(4-methyl-3-phenethyl-piperazin-1-yl)-4H-3-thia-1,4,9-triaza-benzo[f]azulene dihydrochloride | HCID 136360203 | 82.4% |
Reaction Steps
Add a solution of acetyl chloride (0.15 mL, 2.1 mmol) in absolute ethanol at ambient temperature to (S)-2-Butyl-10-(4-methyl-3-phenethyl-piperazin-1-yl)-4H-3-thia-1,4,9-triaza-benzo[f]azulene (0.19 g, 0.41 mmol) in absolute ethanol, with added drops of methanol to solubilize the freebase, and concentrate under reduced pressure gives the title compound (0.18 g). Mass spectrum (APCI+, m/e): 460 (M+1−2HCl); exact mass spectrum (ES+, m/e, C27H33N5S.2HCl): calc. 460.2535 (M+1−2HCl), found 460.2556.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07214673B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-93738a88cf5643f2b01093d19ecd87be |
| Source note | uspto-grants-2007_05 |