HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 9909712, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Methyl (oxolan-2-yl)methyl 2,6-dimethyl-4-(2-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate | HCID 65988 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 9909712 | HCID 9909712 | 79% |
Reaction Steps
To a solution of 30 g (0.07 mol) of 2,6-dimethyl-4-(2-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid 3-methyl ester 5-(tetrahydrofuran-2-ylmethyl) ester in 72 ml of acetic acid, heated to reflux, 7.2 g (0.07 mol) of CrO3 were portionwise added. After the addition was complete, reflux was maintained for one additional hour. The reaction mixture was then slowly poured on ice-cooled aq NH4OH (150 ml). The mixture separated in two phases, and it was evacuated with CH2Cl2 (3×100 ml). The organic extract was dried with anh Na2SO4, and concentrated to dryness at reduced pressure. The resulting oil was crystallised in EtAcO-diethylether, yielding a white solid (mp 69-70° C., EtOH) with a yield of 79%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06482841B1 |
| Source dataset | uspto-grants-2002_11 |
| ORD ID | ord-a90682b1b4b4488e82d0026597ed1fe4 |
| Source note | uspto-grants-2002_11 |