Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus trichloride | HCID 24387 | — |
| Reactant | HCID 20475370 | HCID 20475370 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 20475368 | HCID 20475368 | — |
Reaction Steps
2.1 g (8.1 mmols) of 3-methyl-6-acetoxymethyl-2,2'-bipyridine 1'-oxide are dissolved in 20 ml of benzene at 45° C., and 1.43 g (10.4 mmols) of phosphorus trichloride are added dropwise under an atmosphere of nitrogen. Subsequently, the mixture is boiled under reflux for 30 minutes. After cooling to 23° C., 35 ml of water are added and the benzene phase is separated off. The water phase is washed with twice 15 ml of ethyl acetate. The combined organic phases are dried over sodium sulfate and concentrated in vacuo. After distillation in a bulb tube oven at 125° C./0.13 Pa, 1.51 g (77% of theory) of 3-methyl-6-acetoxymethyl-2,2'-bipyridine are obtained in the form of a colourless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04424359 |
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| Source dataset | uspto-grants-1984_01 |
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| ORD ID | ord-3702a5d3242d4607ad986f756eb61fb3 |
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| Source note | uspto-grants-1984_01 |
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