HuagongsheHuagongshe Chemistry Print Report · For research reference only
Morpholine → 4-(1-Methyl-3,4-dihydroisoquinolin-5-yl)morpholine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | 5-Iodo-1-methyl-3,4-dihydroisoquinoline | HCID 86711315 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4-(1-Methyl-3,4-dihydroisoquinolin-5-yl)morpholine | HCID 86711316 | 44.9% |
Reaction Steps
A flask under Ar was charged with 5-iodo-1-methyl-3,4-dihydroisoquinoline (8.0 g, 29.5 mmol), morpholine (3.1 g, 35.4 mmol) and Cs2CO3 (13.5 g, 41.3 mmol) and a mixture of Pd(OAc)2 (0.33 g, 1.48 mmol) and BINAP (0.92 g, 1.48 mmol) in toluene (150 mL) was added. The reaction was stirred at RT for 5 min and then heated to reflux for 24 h. The reaction was allowed to cool to RT, and then filtered over celite. The filtrate was concentrated in vacuo and the crude product was purified by flash chromatography (SiO2, DCM to DCM/MeOH 9:1) to provide the title compound (3.05 g). UPLC-MS: MS 231.1 (M+H+); UPLC rt 0.40 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853203B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-7018f154a8044e1e921d014b33ab1e58 |
| Source note | uspto-grants-2014_10 |