HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triacetoxyperiodinane → HCID 178493278, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | HCID 178493279 | HCID 178493279 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178493278 | HCID 178493278 | 98.3% |
Reaction Steps
trans-4-[{2-[({[2-chloro-4-(hydroxymethyl)-5-methoxyphenyl]amino}carbonyl)oxy]ethyl}-(methyl)amino]cyclohexyl hydroxy(di-2-thienyl)acetate (intermediate 62; 200 mg; 0.33 mmol) was dissolved in 8 ml dichloromethane and stirred at room temperature in an inert atmosphere. Dess-Martin reagent (170 mg; 0.40 mmol) was added in 3 portions and the reaction stirred for 30 min. Dichloromethane (15 ml) was added, the solution was washed with 4% aqueous sodium hydrogen carbonate solution and vigorously stirred for 1 hour. The solid was filtered and the organic phase of the filtrate was washed with brine, dried and concentrated to give 197 mg of the title compound enough pure to continue with the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09315463B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-883187124a944d1ea10e6e93e38652c7 |
| Source note | uspto-grants-2016_04 |