Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | (R)-2-(tetrahydro-2H-pyran-3-yl)acetaldehyde | HCID 58011477 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 178483677 | HCID 178483677 | 93.2% |
Reaction Steps
To a magnetically stirred solution of (R)-2-(tetrahydro-2H-pyran-3-yl)acetaldehyde (11 g, 85.8 mmol) in Et2O (215 mL) at room temperature was added MeNH2 (2M in THF, 215 mL, 429.2 mmol) and molecular sieves (4 Å, powdered, activated, 21.5 g). The reaction was stirred at room temperature for 1 h. The resulting mixture was then filtered and concentrated under reduced pressure to furnish (R,E)-N-(2-(tetrahydro-2H-pyran-3-yl)ethylidene)methanamine as a yellow oil (11.3 g, 80 mmol, 93%). The crude material was carried on without further purification. 1H NMR (400 MHz, CDCl3) δ 7.67 (m, 1H), 3.86-3.91 (m, 2H), 3.36-3.43 (m, 1H), 3.29 (s, 3H), 3.13 (dd, J=11.0, 9.8 Hz, 1H), 1.95-2.14 (m, 2H), 1.86-1.91 (m, 2H), 1.62-1.68 (m, 2H), 1.21-1.30 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08580823B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-811589d249624ed995d19b1510678e80 |
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| Source note | uspto-grants-2013_11 |
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