HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxylamine → HCID 59556680, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxylamine | HCID 787 | — |
| Reactant | HCID 59556751 | HCID 59556751 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59556680 | HCID 59556680 | 41.2% |
Reaction Steps
Under an atmosphere of nitrogen, (S)-3-chloro-4-(tetrahydrofuran-3-yloxy)benzonitrile (11.2 g, 50.1 mmol) and 50% aqueous hydroxylamine (3.31 g, 50.1 mmol) in EtOH (150.0 mL) was heated at 60° C. for 18 hr. Solvents removed in vacuo and the residue was azeotroped with MeOH. The residual solid was purified by precipitation from an ethyl acetate/30-60° C. pet/ether mixture (1:2) to give (S,Z)-3-chloro-N′-hydroxy-4-(tetrahydrofuran-3-yloxy)benzimidamide (5.3 g) LCMS (Table 1, Method b) Rt=1.52 min, m/z 257.09 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834039B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-79772434eef54b63be52931e1af2fc2b |
| Source note | uspto-grants-2010_11 |