Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Oxygen | HCID 977 | — |
| Reactant | Dimethyl Sulfide | HCID 1068 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Ozone | HCID 24823 | — |
| Reactant | HCID 18466777 | HCID 18466777 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18466701 | HCID 18466701 | — |
Reaction Steps
5,8-Dimethyl-2-(2-furyl)-5,6,7,8-tetrahydroquinoline (3 g) was dissolved in 100 ml of methanol. Ozone generated from oxygen at -78° C. was introduced into the obtained solution for 10 minutes. The resulting system was saturated with nitrogen gas, followed by the addition of 7 ml of dimethyl sulfide. The temperature of the mixture was raised to room temperature and the resulting reaction mixture was concentrated to give about 3 g of a crude product. This crude product containing a carboxylic acid was dissolved in 10 ml of DMF, followed by the addition of 1 ml of methyl iodide and 3.6 g of K2CO3. The obtained mixture was stirred at room temperature for one hour, followed by the addition of 30 ml of water. The obtained mixture was extracted with ethyl acetate (50 ml×2) and the organic phase was washed with a saturated aqueous solution of common salt, dried over MgSO4 and concentrated. The obtained mixture was purified by column chromatography to give 1.6 g of the objective compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06133283 |
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| Source dataset | uspto-grants-2000_10 |
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| ORD ID | ord-945a7d86049441189b5642cb6b6a1033 |
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| Source note | uspto-grants-2000_10 |
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