HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Thiosulfate → Methyl 4-formylcyclohexane-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Cyclohexanecarboxylic acid, 4-(hydroxymethyl)-, methyl ester | HCID 11073869 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 4-formylcyclohexane-1-carboxylate | HCID 11252253 | 99.2% |
Reaction Steps
To a solution of methyl 4-(hydroxymethyl)cyclohexanecarboxylate (Intermediate 87, 4.08 g, 23.7 mmol) in DCM was added NaHCO3 (9.95 g, 118 mmol), followed by Dess-Martin Periodinane (12.1 g, 28.4 mmol). The mixture was stirred at r.t. for 2.5 h. Et2O (60 mL) was added followed by an aq. solution of NaHCO3 (1 M, 60 mL) and a 20% aq. solution of sodium thiosulfate (40 mL). The resulting mixture was stirred overnight. The phases were separated and the aqueous phase was extracted with Et2O. The organic phase was washed with brine and dried over MgSO4, filtered and concentrated in vacuo to yield the title compound (4.0 g, 99% yield): MS (EI) m/z 170 M+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08865911B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-86df18a157ec4625afd815265ab9d306 |
| Source note | uspto-grants-2014_10 |