HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178520509, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 178471154 | HCID 178471154 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178520509 | HCID 178520509 | 90.6% |
Reaction Steps
To a solution of the ester from Step A (120 g, 71.4 mmol) in dry THF (230 mL) at 0° C. was added LAH (2.99 g, 78.6 mmol) portionwise over 30 min. The mixture was stirred for 2 h at room temperature then cooled back to 0° C. and H2O (4.2 mL) was added (care|) dropwise. This was followed by the dropwise addition of 10.6 mL of 1N NaOH then the resulting slurry was stirred at room temperature for 1 h. After filtration through celite washing with EtOAc, the solvent was removed to give the title compound as a clear oil (8.16 g). 1H NMR (CD3OD): δ 1.84 (2H, pentet), 2.68 (2H, t), 3.58 (2H, t), 6.88 (1H, s), 7.80 (1H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05856326 |
| Source dataset | uspto-grants-1999_01 |
| ORD ID | ord-0964826ae62c4609bf17029ace9192c6 |
| Source note | uspto-grants-1999_01 |