Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 7-Benzyl-8-chloro-1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione | HCID 325372 | — |
| Reactant | HCID 14999084 | HCID 14999084 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 10293403 | HCID 10293403 | 97% |
Reaction Steps
[1,4]Diazepan-6-ol acetate (2B) (116 mg, 0.49 mmol) and 7-benzyl-8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione (100 mg, 0.33 mmol) were dissolved in 2-propanol (20 ml) and triethylamine (0.68 ml, 4.9 mmol) and the mixture was subjected to micro waves (150° C., 6 bar, 300 W, 8 hours). The solvents were evaporated and the remaining was redissolved in dichloromethane (20 ml) and water (20 ml). The aqueous layer was acidified with potassium hydrogen sulfate until pH=2. The aqueous layer was separated and aqueous sodium hydroxide was added until pH=12. The aqueous layer was extracted with 3×50 ml of dichloromethane, and the combined organic material were added excess trifluoroacetic acid, and evaporated, to afford 123 mg of the title compound as a brown oil in 75% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07235538B2 |
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| Source dataset | uspto-grants-2007_06 |
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| ORD ID | ord-9b6c61b507f94d2a93aca72cc5066565 |
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| Source note | uspto-grants-2007_06 |
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