HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178521618, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3-(4-Bromophenyl)cyclobutan-1-one | HCID 4589695 | — |
| Reactant | Ammonium chloride monohydrate | HCID 57429219 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178521618 | HCID 178521618 | 66.6% |
Reaction Steps
At −78° C., 1.0 M tri(tert-butoxy)lithiumaluminium hydride (24 mL, 24 mmol) was added to a THF (20 mL) solution of 3-(4-bromophenyl)cyclobutanone (4.53 g, 20.1 mmol), and stirred at the same temperature for 1.5 hours. Saturated ammonium chloride water and 1 N hydrochloric acid were added to the reaction liquid, extracted with ethyl acetate, dried with anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure, the obtained residue was purified by silica gel column chromatography (C-200, ethyl acetate:hexane=1:4 to 3:7) to obtain the entitled compound (3.04 g, 66%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07875633B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-ffd1d72c1d7a4c14a619a620f99ba6ee |
| Source note | uspto-grants-2011_01 |