HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 12085085, compound → HCID 12085086, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 12085085 | HCID 12085085 | — |
| Reactant | Pyridiniumtribromide | HCID 21124087 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12085086 | HCID 12085086 | — |
Reaction Steps
A solution of Example 27B (4.03 g, 14.54 mmol) in THF (200 mL) at room temperature was treated over 15 minutes with pyridinium tribromide (5.16 g, 15.26 mmol), stirred for 14 hours, and concentrated. The concentrate was treated with water (200 mL), stirred at room temperature for 15 minutes, and filtered. The resulting solid was washed with water (200 mL), suspended in hot CH3CN, cooled to room temperature, and filtered to provide a first crop of desired product. The filtrate was treated with charcoal, filtered, and concentrated to provide a solid which was suspended in diethyl ether and filtered to provide a second crop of desired product. MS (ESI(−)Q1MS) m/z 355 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06329534B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-e0527eab1048462a96da13e4c25329fd |
| Source note | uspto-grants-2001_12 |