Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Reactant | HCID 11084758 | HCID 11084758 | — |
| Reactant | HCID 178418373 | HCID 178418373 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 23345447 | HCID 23345447 | 83% |
Reaction Steps
Under an argon atmosphere, 0.54 g of magnesium turnings (22 mg atom) was mixed with dry diethylether (15 ml), and 3.72 g of methyl iodide (93% purity, 24 mmol) solution in dry diethylether (15 ml) was dropped gradually thereto to prepare Grignard reagent of methylmagnesium iodide. The Grignard reagent was gradually added in drop-wise into 3.60 g of 2-(dichloroacetyl)thiophene (18.5 mmol) solution in dry diethylether (15 ml) with cooling in an ice-water bath so as to maintain a temperature below 10° C. After the dropwise addition was completed, the reaction mixture was agitated over a night at room temperature, and then, 20 ml of a saturated aqueous solution of ammonium chloride was added thereto and extracted with ether. The ether layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate and the ether was distilled off. Thus, 1-(2-thienyl)-1-dichloromethylethanol was obtained in an amount of 3.22 g (yield 83%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04219659 |
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| Source dataset | uspto-grants-1980_08 |
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| ORD ID | ord-8596a73099224817a681e0e0f008b865 |
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| Source note | uspto-grants-1980_08 |
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