HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → [4-(Cyclopropylcarbonyl)pheny]methyl-propanedioic acid, dimethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Dimethyl Carbonate | HCID 12021 | — |
| Reactant | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| Reactant | Methyl 2-(4-(cyclopropanecarbonyl)phenyl)acetate | HCID 12096482 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | [4-(Cyclopropylcarbonyl)pheny]methyl-propanedioic acid, dimethyl ester | HCID 67524057 | 21.1% |
Reaction Steps
Dissolve 4-(cyclopropylcarbonyl)benzeneacetic acid, methyl ester (1.5 g, 6.0 mmol) and dimethylcarbonate (930 mg, 10.3 mmol) in tetrahydrofuran (10 mL). Add 20 mL (20 mmol) of a 1.0 molar solution of sodium bis(trimethylsilyl)amide in tetrahydrofuran over 0.5 hours. Stir 3 days. Add iodomethane (5.3 g, 35 mmol). Stir 24 hours. Add water and ethyl acetate. Wash organic phase with brine, dry over anhydrous magnesium sulfate and concentrate. Purify by flash chromatography (50 g silica gel, ethyl acetate/heptane as eluent) to give the title compound (315 mg, 16%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06700012B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-ef6ce2a02caa4769ae002aeff9a27a6a |
| Source note | uspto-grants-2004_03 |