HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86590126, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 22671391 | HCID 22671391 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86590126 | HCID 86590126 | — |
Reaction Steps
At −20° C., under an atmosphere of protective gas, 3 mmol of a 1-molar solution of LiAlH4 in tetrahydrofuran (THF) were added dropwise to a solution of 0.86 g of 5-chloro-2-hydroxy-6,6′-dimethyl-2′, 3′, 4′-trimethoxybenzophenone in 10 ml of anhydrous THF. The reaction mixture was warmed to room temperature and then admixed with ice water, acidified with dilute hydrochloric acid and extracted with ethyl acetate. The combined organic phases were washed with sat. NaCl solution, dried and purified by column chromatography (mobile phase: ethyl acetate/cyclohexane 3:7). This gave 0.46 mg of the title compound as a white solid of m.p. 140-142° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06767923B2 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-9f08fd0f06994c039fc350a342f3ba72 |
| Source note | uspto-grants-2004_07 |