HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23130698, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 23130686 | HCID 23130686 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23130698 | HCID 23130698 | 85.2% |
Reaction Steps
3-(3-Methyl-2-butenyloxy)-benzonitrile described in Preparation Example 133 (1.71 g, 10 mmol) was dissolved in tetrahydrofuran (20 mL), lithium aluminum hydride (0.57 g, 15 mmol) was added under stirring at room temperature, the solution was heated to 70° C., then stirring continued for 2 hours. The reaction solution was cooled on an ice bath, then, water (0.6 mL), an aqueous solution of 15% sodium hydroxide (0.6 mL) and water (1.8 mL) were added in this order, then, the solid was filtered, and washed with tetrahydrofuran (20 mL). The filtrate and the washings were combined, and dried over anhydrous sodium sulfate. The solvent was evaporated in vacuo, and the title compound (1.50 g, 8.52 mmol, 85.2%) was obtained as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07932272B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-890b540f9b4040d4aa11a0cc7ceaa950 |
| Source note | uspto-grants-2011_04 |