HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenesulfonyl chloride → HCID 67241199, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenesulfonyl chloride | HCID 7369 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 67241493 | HCID 67241493 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67241199 | HCID 67241199 | 16.5% |
Reaction Steps
Sodium hydride (60% in mineral oil, 14 mg, 0.54 mmol, 95%) was added to a solution of 2,7-dimethyl-1,3,4,8-tetrahydro-2H-[1,4]oxazepino[6,7-e]indole trifluoroacetate (Intermediate 13, 0.060 g, 0.18 mmol) in DMF (2 mL) and stirred at room temperature for 5 minutes before benzenesulfonyl chloride (0.035 mL, 0.27 mmol) was added. The mixture was stirred at room temperature for 10 minutes and quenched with ice/water and extracted with DCM. The crude material was purified by preparative HPLC (ACE C8, 0.1% TFA-CH3CN) to give the title compound as a brown oil (14 mg) in the form of the trifluoroacetate salt. MS m/z 357 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07960374B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-60cc3136039f49cf83752352daa858b8 |
| Source note | uspto-grants-2011_06 |