HuagongsheHuagongshe Chemistry Print Report · For research reference only
4,4-Dimethyl-7-nitro-3,4-dihydroisoquinolin-1(2H)-one → 4,4-Dimethyl-7-nitro-1,2,3,4-tetrahydroisoquinoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4,4-Dimethyl-7-nitro-3,4-dihydroisoquinolin-1(2H)-one | HCID 14209953 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4,4-Dimethyl-7-nitro-1,2,3,4-tetrahydroisoquinoline | HCID 21959655 | — |
Reaction Steps
4,4-Dimethyl-7-nitro-3,4-dihydro-2H-isoquinolin-1-one (230 mg) was dissolved in THF (10 ml) and BH3Me2S (400 ul) was added and the reaction was stirred overnight at RT. The reaction was quenched with MeOH (10 ml) and NaOH (200 mg) and heating at reflux for 20 min. The mixture was extracted with EtOAc, washed with sat'd NH4Cl, extracted with 10% HCl (20 ml). The acidic solution was treated with 5N NaOH (15 ml), extracted with EtOAc (30 ml) dried, filtered and evaporated to give the compound as a yellow solid. M+H 207.2, Calc'd 206.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08642624B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-67a10b7e348248cbb501dc5e6d51a5f0 |
| Source note | uspto-grants-2014_02 |