Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 5-hydroxymethyl-N-methyl-N-propyl-isophthalamic acid ethyl ester | HCID 68816479 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86615013 | HCID 86615013 | 91% |
Reaction Steps
Add a solution of 5-hydroxymethyl-N-methyl-N-propyl-isophthalamic acid ethyl ester (600 mg, 2.15 mmol) dropwise to a mixture of Dess-Martin periodinane (1.06 g, 2.5 mmol) in dichloromethane (6.5 mL). Stir the exothermic reaction mixture (32° C.) for 20 min without additional heat. To the reaction mixture add diethyl ether (12 mL) and saturated aqueous sodium bicarbonate (12 mL). Separate the layers and wash the aqueous layer with diethyl ether (2×12 mL). Combine the organics and wash with saturated aqueous sodium bicarbonate (12 mL), saturated aqueous sodium chloride (12 mL), dry (magnesium sulfate), concentrate, and purify (silica gel chromatography, eluting with 50:50 ethyl acetate:hexanes) to give the title compound as an oil (0.54 g, 91%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07585885B2 |
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| Source dataset | uspto-grants-2009_09 |
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| ORD ID | ord-62320f7b3a914087bc12cfb79925fa21 |
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| Source note | uspto-grants-2009_09 |
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