Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitromethane | HCID 6375 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | 4-(2-(Tetrahydrofuran-2-yl)-ethyl)-benzaldehyde | HCID 59255341 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 59255150 | HCID 59255150 | 94.3% |
Reaction Steps
To an acetic acid (10 mL) solution of 4-(2-(tetrahydrofuran-2-yl)-ethyl)-benzaldehyde (565 mg, 2.77 mmol) described in Manufacturing Example 82-1-3 were added nitromethane (1.69 g, 27.7 mmol) and ammonium acetate (427 mg, 5.54 mmol) under nitrogen atmosphere at room temperature, which was stirred for 4 hours at 120° C. The reaction mixture was partitioned into water and ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure to obtain the title compound (646 mg, 94%) as a crude product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07691882B2 |
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| Source dataset | uspto-grants-2010_04 |
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| ORD ID | ord-354c1d3071734465a0f5ee589a53e2cf |
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| Source note | uspto-grants-2010_04 |
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