HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 10364529, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 68870373 | HCID 68870373 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10364529 | HCID 10364529 | 89.1% |
Reaction Steps
Lithium hydroxide (14.4 mg, 0.6 mmol) dissolved in water (1 ml) was added into 70377 methyl 2-({4-[3-(3,4-dihydroisoquinolin-2(1H)-yl)-3-oxopropyl]phenoxy}methyl)benzoate (129 mg, 0.3 mmol) in THF (2 ml). The mixture was put in a microwave oven (Smith Synthesizer) and irradiated at 150° C. for 7 minutes and then evaporated to remove THF. The residue was acidified with 1% hydrochloric acid, pH˜5, and extracted with ethyl acetate (×2). The extracts were combined and dried (magnesium sulphate) and evaporated. Chromatography of the residue on a column (ISOLUTE® SI, 2 g/6 ml) using DCM, MeOH/DCM (1:99) as eluant gave 111 mg the desired product yield 89%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07521461B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-485161a4f2da45a48d2ad1a7b0e55d11 |
| Source note | uspto-grants-2009_04 |