HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 178473734, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 178477855 | HCID 178477855 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178473734 | HCID 178473734 | 68% |
Reaction Steps
To a solution of trans-1-(4-benzo[d]isothiazol-3-yl-cyclohexyl)-8-chloro-5,6-dihydro-4H-2,3,5,10b-tetraaza-benzo[e]azulene (35 mg, 0.080 mmol) and triethylamine (0.022 ml, 0.16 mmol) in dichloromethane (0.8 ml) was added acetyl chloride (0.011 ml, 0.16 mmol) at room temperature. Stirring for 20 h was followed by partitioning between water (20 ml) and ethyl acetate (25 ml). The layers were separated. The organic layer was washed with two 25 ml-portions of water. The organic layer was concentrated in vacuo. Preparative RP-HPLC with water (0.05% formic acid)/methanol as eluent gave the title compound (26 mg, 68%) as white solid. MS m/e: 478 ([M+H]+)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481528B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-086aacda821541dcaa2d2dd9fedbcefb |
| Source note | uspto-grants-2013_07 |