HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Hydroxide → HCID 67429636, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 4-Bromoheptane | HCID 70460 | — |
| Reactant | HCID 10061724 | HCID 10061724 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 67429636 | HCID 67429636 | 117.5% |
Reaction Steps
0.2 g of 5-iodo-2H-isoquinolin-1-one, 234 mg of 4-bromoheptane, 62 mg of finely ground potassium hydroxide, 79 mg of tetrabutylammonium bromide then 28 cm3 of toluene are stirred, under an inert atmosphere, for 6 h at the reflux of the solvent. The reaction mixture is filtered through sintered glass. The filtrate is concentrated using a rotary evaporator under reduced pressure (5 kPa). The 320 mg of brown oil obtained are purified by flash chromatography over silica (column: 35 g; particle size: 20-40 μm, spherical; eluent: 80% heptane/20% ethyl acetate). After concentrating the fractions under reduced pressure, 165 mg of 5-iodo-2-(1-propylbutyl)isoquinolin-1(2H)-one are obtained in the form of a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08030320B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-eaafd86223054660b2789489ef94315e |
| Source note | uspto-grants-2011_10 |