Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Carbonochloridic acid, heptyl ester | HCID 118547 | — |
| Reactant | HCID 178526940 | HCID 178526940 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 19773971 | HCID 19773971 | 83% |
Reaction Steps
100 ml of chloroform and 7.3 ml (0.052 mol) of triethylamine were added to 4.5 g (0.040 mol) of 4-hydroxypyridine monohydrate to dissolve it, and the solution was stirred at 25° C. 8.9 g (0.050 mol) of heptyl chlorocarbonate was added to the solution dropwise. After stirring for 30 min, cold aqueous hydrochloric acid was added thereto. After separation the resulting chloroform layer was washed twice with cold water and then dried over Glauber's salt. After filtering out the Glauber's salt, the chloroform was removed by distillation, and the obtained product was purified by column chromatography, followed by crystallization from ethanol, thereby obtaining 7.5 g of exemplified compound I-24 having a melting point of 44° to 50° C. in a yield of 83%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05098805 |
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| Source dataset | uspto-grants-1992_03 |
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| ORD ID | ord-655a35be62bf42cab8f93d7b6db8717a |
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| Source note | uspto-grants-1992_03 |
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