Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Homoallyl bromide | HCID 21241 | — |
| Reactant | 3-Methylxanthine | HCID 70639 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 13298149 | HCID 13298149 | — |
Reaction Steps
41.5 g of 3-methyl-xanthine are added with stirring at 70° C. to a solution of 10.2 g of NaOH in 400 ml of methanol/water (1:1). After mixing with 35.1 g of 4-bromobut-1-ene the mixture is stirred under a nitrogen atmosphere for 27 hours at 70° C. The reaction mixture is then cooled to 20° C. and the precipitate formed is filtered off. By re-precipitation from alkaline solution (pH 13.5) and acidification with dilute sulphuric acid to pH 10, 29.6 g (89.7% of theory relative to reacted 3-methyl-xanthine) of the title compound of melting point 245° to 246° C. are obtained after drying.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04207321 |
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| Source dataset | uspto-grants-1980_06 |
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| ORD ID | ord-6735627665dc46b8ba6531aa743edf87 |
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| Source note | uspto-grants-1980_06 |
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