Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 10775307 | HCID 10775307 | — |
| Reactant | Ethyl acetate hexane | HCID 21226206 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 187401-16-7 | HCID 10751321 | 87.8% |
Reaction Steps
A solution of 7.7 g of 5,6,7,8-tetrahydro-5,5,8,8-tetramethylquinoxaline-2-methanol in 120 ml of dichloromethane was then added dropwise to the reaction mixture and the resulting mixture-was stirred for 15 minutes. To the reaction mixture were added with 35.1 ml of triethylamine, followed by stirring for 5 minutes. After the reaction mixture was raised to room temperature and stirred for 15 minutes, water was added and the resulting mixture was extracted with dichloromethane. The organic layer was successively washed with water and saturated saline, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue so obtained was subjected to chromatography on a silica gel column (developing solvent: 10% ethyl acetate/n-hexane), whereby 6.7 g of the title compound were obtained as a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06630463B2 |
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| Source dataset | uspto-grants-2003_10 |
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| ORD ID | ord-efa73725d91249bd92cc3b48f471ee1a |
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| Source note | uspto-grants-2003_10 |
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