Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 23509657 | HCID 23509657 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23509648 | HCID 23509648 | — |
Reaction Steps
The product of example 1b above, 2-phenylamino-6-phenylbenzonitrile, (0.13 g, 0.48 mmol) was dissolved in dry tetrahydrofuran (20 mL) and stirred under argon in a room temperature water bath. Lithium aluminum hydride (0.182 g, 4.8 mmol) was added rapidly. After 5 minutes at room temperature the reaction mixture was heated to 60° C. for 2 hours. The reaction mixture was cooled to room temperature and anhydrous sodium sulfate was added followed by the addition of a freshly prepared saturated solution of anhydrous sodium sulfate. The solvent was evaporated and the residue triturated with ethyl acetate, filtered and evaporated. Flash chromatography on silica gel eluted with 0-2% methanol in methylene chloride gave the title compound as a white amorphous solid. mp 115-116° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06759410B1 |
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| Source dataset | uspto-grants-2004_07 |
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| ORD ID | ord-d73d66756be94823b76d19c61ba7a9ec |
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| Source note | uspto-grants-2004_07 |
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