HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 18348544, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 2,6-Pyridinedicarboxylic acid | HCID 10367 | — |
| Reactant | Ceric ammonium nitrate | HCID 180504 | — |
| Reactant | HCID 18348662 | HCID 18348662 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18348544 | HCID 18348544 | 79.6% |
Reaction Steps
To a mixture of 7-[2-(4-chlorophenoxy)ethyl]-1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cycloheptene (1.38 g), 2,6-pyridinedicarboxylic acid (1.64 g), THF (52 ml), and water (13 ml) was dropwise added a solution of CAN (7.18 g) in water (13 ml) with cooling with ice. After the reaction mixture was stirred for 15 min, water was added to the reaction mixture, which was extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and dried. The solvent was removed in vacuo. The residue was purified by alumina column chromatography(ethyl acetate) and then with recrystallization from hexane-ethyl acetate to yield the entitled compound (1.02 g) as crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06326369B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-407a9b54d0b245af95fcd3e9c7d9b3c7 |
| Source note | uspto-grants-2001_12 |