HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 25183370, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 59180453 | HCID 59180453 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 25183370 | HCID 25183370 | 94.6% |
Reaction Steps
To a solution of 11 (24.7 mL; 0.06 mmol) in tetrahydrofuran (5 mL) in a 2.5-5.0 mL microwave reactor tube was added aqueous lithium hydroxide (1 mL; 2M). The reaction vessel was subjected to the following microwave conditions: Temperature=140° C.; Time=15 minutes; Power=250 W; Cooling on; Absorption=Very High. The crude reaction mixture was allowed to cool to room temperature, acidified by the addition of aqueous hydrochloric acid (15 mL; 2N), and extracted with ethyl acetate (3×10 mL). The organic phases were combined and dried over magnesium sulfate, filtered, and concentrated under reduced pressure to afford a beige solid. The latter was triturated from diisopropyl ether to yield the title compound as a beige solid (24.1 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178699B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-416cabbc037f4ba3baf4ae5b5f4f87ee |
| Source note | uspto-grants-2012_05 |