HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl azide → HCID 136384027, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl azide | HCID 12152 | — |
| Reactant | Sodium Ascorbate | HCID 23667548 | — |
| Reactant | HCID 136413571 | HCID 136413571 | — |
| Solvent | Dichloromethane ethanol | HCID 21584144 | — |
| Product | HCID 136384027 | HCID 136384027 | 76.7% |
Reaction Steps
To a mixture of 3-(4-chloro-phenyl)-7-ethynyl-4-hydroxy-isothiazolo[5,4-c]pyridine-5-carboxylic acid ethyl ester (0.106 mmol) and CH2Cl2/H2O (1/1, 0.70 mL) was added benzylazide (0.117 mmol), CuSO4.5H2O (0.0053 mmol) and sodium L-ascorbate (0.0159 mmol). The mixture was stirred at rt for 16 h before it was partitioned between H2O (20 mL) and CH2Cl2 (20 mL). The aqueous phase was then extracted with CH2Cl2 (2×15 mL). The combined organic layers were washed with brine and water, dried over MgSO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel, eluting with 0-20% EtOAc/CH2Cl2, to give the title compound (40 mg) as a white solid: MS (m/z) 492.1 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08952160B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-1af8a708e7b6435d92151c5ba4275f62 |
| Source note | uspto-grants-2015_02 |