Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 87577134 | HCID 87577134 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 87576195 | HCID 87576195 | — |
Reaction Steps
To a mixture of 0.68 g (0.0022 mole) of (rac)-6-chloro-4-cyclopentyl-2,3,3a,4,9,10a-hexahydro-1H-4,5,7,9-tetraaza-benzo[f]azulen-10-one (VI-68), 20 mL of dimethylformamide and 1.83 g (0.0056 mole) of cesium carbonate was added 1.254 g (0.0088 mole) of iodomethane. The mixture was stirred for 20 minutes, then diluted with ethyl acetate and water. The water layer was extracted twice with ethyl acetate and the combined ethyl acetate layers washed successively with water, then brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to give 0.580 g of (rac)-6-chloro-4-cyclopentyl-9-methyl-2,3,3a,4,9,10a-hexahydro-1H-4,5,7,9-tetraazabenzo[f]azulen-10-one (VII-68), which was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07517873B2 |
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| Source dataset | uspto-grants-2009_04 |
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| ORD ID | ord-efe5a3dbbf8f42418d3629eafb09cfc7 |
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| Source note | uspto-grants-2009_04 |
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