Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | 3-Chloro-6-methylpyridazine | HCID 227254 | — |
| Reactant | HCID 86654078 | HCID 86654078 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86654080 | HCID 86654080 | — |
Reaction Steps
A mixture of cis-10-hydroxy-2,3,4a,5,6,10b-hexahydro-1H-benzo[f]quinoline-4-carboxylic acid tert-butyl ester (0.40 g), 3-chloro-6-methyl-pyridazine (0.13 g), cesium carbonate (0.35 g), and N-methylpyrrolidinone (5 mL) is stirred at 150° C. for 1.5 h. After cooling to room temperature, the mixture is diluted with ethyl acetate and washed with water and brine and dried (Na2SO4). The solvent is evaporated and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 3:1→1:2) to give the title compound. Yield: 0.14 g (impure); LC (method 1): tR=4.19 min; Mass spectrum (ESI+): m/z=396 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09120769B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-97785f3020b143c39366a7a53a43de41 |
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| Source note | uspto-grants-2015_09 |
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