HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → [4-(Cyclopropylcarbonyl)phenyl]methyl-propanedioic acid, diethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Diethyl Carbonate | HCID 7766 | — |
| Reactant | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| Reactant | Ethyl 2-(4-(cyclopropanecarbonyl)phenyl)acetate | HCID 11218514 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | [4-(Cyclopropylcarbonyl)phenyl]methyl-propanedioic acid, diethyl ester | HCID 12132442 | 26.4% |
Reaction Steps
Dissolve 4-(cyclopropylcarbonyl)benzeneacetic acid, ethyl ester (6.5 g, 28 mmol) and diethylcarbonate (4.0 g, 34 mmol) in tetrahydrofuran (100 mL). Add 62 mL (62 mmol) of a 1.0 molar solution of sodium bis(trimethylsilyl)amide in tetrahydrofuran over 0.5 hours. Stir 28 hours. Add iodomethane (5.3 g, 35 mmol). Stir 2 days. Add water and ethyl acetate. Wash organic phase with brine, dry over anhydrous magnesium sulfate and concentrate. Purify by flash chromatography (200 g silica gel, ethyl acetate/heptane as eluent) to give the title compound (1.43 g, 17%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06930197B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-90308ffcf50043f1a75ee0e6db60cb39 |
| Source note | uspto-grants-2005_08 |