HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 12113148, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2,3-Dihydro-2,3,3-trimethyl-1H-inden-1-one | HCID 10149036 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12113148 | HCID 12113148 | 98.7% |
Reaction Steps
3,3,2-Trimethyl-1-indanone (9.03 g, 50 mmol) as prepared above was dissolved in THF (40 ml) and added to the suspension of LiAlH4 (3.80 g, 100 mmol, 2 equiv.) in THF (10 ml). The mixture was heated to reflux for 2 h, then cooled to 5° C. and hydrolysed via addition of 2N aq. HCl-solution. The crude product obtained after extraction with MTBE, washing with sat. aq. NaHCO3 solution and brine, drying over MgSO4 and concentrating in a rotary evaporator was distilled at 0.1 mbar/72-73° C. to yield 8.70 g (95%) of product as a colourless viscous oil. The compound was obtained as a mixture of diastereomers 87:13, the major isomer being the 1,2-trans compound upon NMR-analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07538243B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-45481bfcaefe4bbc9134f160d1ea21c6 |
| Source note | uspto-grants-2009_05 |