Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | N,N-Dimethylaminoethyl chloride hydrochloride | HCID 11636816 | — |
| Reactant | HCID 20670051 | HCID 20670051 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 20670032 | HCID 20670032 | — |
Reaction Steps
A mixture of the amino compound from Example 54 (0.10 g), potassium carbonate (0.087 g) and N-(2-chloroethyldimethylamine hydrochloride was stirred and heated at 138° C. for 72 hr. The residue was dissolved in water and the product extracted into ethyl acetate. The organic extract was washed with brine, dried over sodium sulphate (Na2SO4) and concentrated to give an oil which was purified by Supercritical Fluid Chromatography eluting with CO2/methanol/0.1% diethylamine to give an oil. Addition of excess ethereal hydrogen chloride solution gave a solid which was triturated under an ether/ethanol/dichloromethane mixture to give a colourless powder (0.04 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06201024B1 |
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| Source dataset | uspto-grants-2001_03 |
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| ORD ID | ord-32fae5d0ba884003b6d060c2b6cf9794 |
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| Source note | uspto-grants-2001_03 |
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