Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclohexylamine | HCID 7965 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 1-Chloro-4-(4-pyridinylmethyl)phthalazine | HCID 1944609 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22741972 | HCID 22741972 | 0.56% |
Reaction Steps
A mixture of 0.3 g (1.173 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.523 g (5.278 mmol) cyclohexylamine is stirred for 8 h at 115° C. The cooled reaction mixture is then distributed between dichloromethane and saturated aqueous sodium hydrogen carbonate solution. The organic solution washed with brine and dried over anhydrous sodium sulfate is evaporated and the residue purified on silica gel by flash chromatography using acetate/methanol (19:1). Title compound (with water content of 0.56%) is obtained after crystallization of the product-containing fractions from acetonitrile and drying under HV; m.p. 137-139° C.; ESI-MS: (M+H)+=319.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06258812B1 |
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| Source dataset | uspto-grants-2001_07 |
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| ORD ID | ord-c9fd1a902bec43908d03b578d5fc8fb5 |
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| Source note | uspto-grants-2001_07 |
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