HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23130535, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 23130374 | HCID 23130374 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23130535 | HCID 23130535 | 91.1% |
Reaction Steps
5-(2-Methylpropenyl)-thiophene-2-carbonitrile described in Preparation Example 144 (15 mg, 0.092 mmol) was dissolved in tetrahydrofuran (2 mL), lithium aluminum hydride (10 mg, 0.26 mmol) was added under stirring at room temperature, the solution was heated to 70° C., followed by stirring for 2 hours. The reaction solution was cooled on an ice bath, then, water (0.01 mL), an aqueous solution of 15% sodium hydroxide (0.01 mL) and water (0.03 mL) were sequentially added, then, the solid was filtered, and washed with tetrahydrofuran (5 mL). The filtrate and the washings were combined, and dried over anhydrous sodium sulfate. The solvent was evaporated in vacuo, and the title compound (14 mg, 0.083 mmol, 91.1%) 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-dc0f40ed58884193ae6e32006ce0eaac |
| Source note | uspto-grants-2011_04 |