HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetaldehyde → O-benzyl-N-vinyl-hydroxylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetaldehyde | HCID 177 | — |
| Reactant | Benzyloxyamine hydrochloride | HCID 102312 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | O-benzyl-N-vinyl-hydroxylamine | HCID 57227192 | — |
Reaction Steps
Acetaldehyde (24.7 mL, 44.2 mmol) was added dropwise to the cooled solution (0° C.) of O-benzyl-hydroxylamine hydrochloride (7.00 g, 43.85 mmol) in water (100 mL) and MeOH (20 mL). The reaction mixture was stirred for 16 h. The volatiles were removed under reduced pressure, and the water suspension was extracted with EtOAc (2×75 mL). The combined organic extracts were washed with brine, and then dried over Na2SO4 and evaporated to yield O-benzyl-N-vinyl-hydroxylamine (LXVI) in quantitative yield. 400 MHz 1H NMR (DMSO-d6, ppm) 7.48 (0.5H, q, J=5.8 Hz), 7.39-7.26 (5H, m), 6.86 (0.5H, q, J=5.5 Hz), 5.06 (1H, s), 4.97 (1H, s), 1.78 (1.5H, d, J=5.5 Hz), 1.76 (1.5H, d, J=5.8 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09162992B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-c4352ac75c404dd5acae3a350dd23f81 |
| Source note | uspto-grants-2015_10 |