HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → (NE)-N-[[3,3-bis(fluoromethyl)-1-hydroxy-2,1-benzoxaborol-5-yl]methylidene]hydroxylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 3,3-Bis(fluoromethyl)-1-hydroxy-1,3-dihydrobenzo[c][1,2]oxaborole-5-carbaldehyde | HCID 86685075 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (NE)-N-[[3,3-bis(fluoromethyl)-1-hydroxy-2,1-benzoxaborol-5-yl]methylidene]hydroxylamine | HCID 89572707 | — |
Reaction Steps
To a mixture of 3,3-bis(fluoromethyl)-1-hydroxy-1,3-dihydrobenzo[c][1,2]oxaborole-5-carbaldehyde (400 mg, 1.77 mmol) and NH2OH.HCl (148 mg, 2.12 mmol) in THF (25 mL) and H2O (5 mL) at rt was added NaOAc (203 mg, 2.48 mmol). The mixture was stirred at rt overnight, diluted with H2O and extracted with EA (50 mL×2). The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The crude product (440 mg) was used directly in the next step without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09156860B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-34b8ac48961b49f1b78a0d76597ae4f1 |
| Source note | uspto-grants-2015_10 |