Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 19013279 | HCID 19013279 | — |
| Solvent | Cyclohexane | HCID 8078 | — |
| Product | HCID 19013275 | HCID 19013275 | — |
Reaction Steps
8.76 g (22.66 mmol) of 2-[[2-[4-(2,5-dimethoxyphenyl) piperazin-1-yl]ethyl]amino]pyrimidine-4-carboxamide are introduced into 650 ml of methanol in a 1 l round-bottomed flask, a stream of gaseous hydrochloric acid is passed through for a few minutes and the mixture is then heated at the reflux temperature of the methanol for 5 h. The solventis evaporated under reduced pressure, 300 ml of dichloromethane are added to the residue and the mixture is then basified with a saturated aqueous sodium hydrogencarbonate solution. The organic phase is dried over sodium sulphate, filtered and the solvent is then evaporated under reduced pressure. After purification by chromatography on a silica gel column (eluent: 100/0 to 90/10 dichloromethane/methanol mixture) and then by recrystallisation from cyclohexane, 6.93 g (17.26 mmol) of ester are isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05330985 |
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| Source dataset | uspto-grants-1994_07 |
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| ORD ID | ord-b678ec4ed35649babc7ee6263316ec03 |
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| Source note | uspto-grants-1994_07 |
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