HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dimethoxyethane → 5-(4-Chlorophenyl)-N-methyl-8-nitro-1,2,3,4-tetrahydroisoquinoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dimethoxyethane | HCID 8071 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 4-Chlorophenylboronic acid | HCID 74299 | — |
| Reactant | 5-Bromo-2-methyl-8-nitro-1,2,3,4-tetrahydroisoquinoline | HCID 10016010 | — |
| Solvent | Water | HCID 962 | — |
| Product | 5-(4-Chlorophenyl)-N-methyl-8-nitro-1,2,3,4-tetrahydroisoquinoline | HCID 23435821 | — |
Reaction Steps
A mixture of 5-bromo-N-methyl-8-nitro-1,2,3,4-tetrahydroisoquinoline (4.07 g, 15 mmol), 4-chlorophenylboronic acid (3.5 g, 22.5 mmol), sodium carbonate (8.0 g, 75.5 mmol), 1,2-dimethoxyethane (60 ml), water (30 ml) and tetrakis(triphenyl-phosphine)palladium(0) (0.20 g, 0.17 mmol) was stirred at reflux for 3.5 h. Water (50 ml) was added and the mixture was extracted with ethyl acetate (100 ml). The crude mixture was recrystallized from ethanol (96%). Yield 3.62 g (80%). Mp 162-163° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07595336B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-3b181741bc2a4b5588d658cebb7ad6ab |
| Source note | uspto-grants-2009_09 |