Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Theobromine | HCID 5429 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 23287948 | HCID 23287948 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 15230636 | HCID 15230636 | 97.1% |
Reaction Steps
Theobromine (3.45 g, 19.2 mmol) was added to a suspension (30 ml) of sodium hydride (461 mg, 19.2 mmol) in dimethylsulfoxide. After 15 minutes, the 9-decenylmesylate (2.25 g, 11 mmol) was added and the reaction stirred for 18 hours at 25° C., then for 40 minutes at 100° C. The mixture was then poured into water (100 ml) and extracted with three 50 ml aliquots of dichloromethane. The combined organic portions were washed with saturated salt solution (60 ml) and dried over magnesium sulfate. Evaporating the solvent under vacuum left a white solid residue. Recrystallization of the residue in ether produced 3.40 g of 1-(9-decenyl)-3,7-dimethylxanthine (56% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06043250 |
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| Source dataset | uspto-grants-2000_03 |
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| ORD ID | ord-496f46c088a140cd9aa01f63438ee37b |
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| Source note | uspto-grants-2000_03 |
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