HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68890297, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 68889281 | HCID 68889281 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 68890297 | HCID 68890297 | 100.3% |
Reaction Steps
(R)-4-Methyl-7-trifluoromethyl-3,4-dihydro-2H-pyrazino[1,2-a]indol-1-one (2.75 g; 10 mmol) was dissolved in diethylether (200 mL) and lithium aluminium hydride (0.78 g, 21 mmol) was added in portions with cooling. The solution was stirred for 2 h at reflux temperature, cooled and hydrolyzed by sequential addition of water (3.0 mL), sodium hydroxide solution (15%, 6.0 mL) and water (6.0 mL). Diethylether was added (100 mL), the mixture was filtered and the filtrate evaporated. The residue was stirred with hexane (20 mL) and diethylether (1 mL) to give the title compound as white solid (2.55 g, 97%). M.p.: 123–125° C., ISP-MS: m/e=255.1 (M+), αD20=−110.0
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07253281B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-10116726bf3b4ef282110fba882217c8 |
| Source note | uspto-grants-2007_08 |