HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → (R)-1-(5-acetoxyhexyl)-8-(2-chloroethylamino)-3-methylxanthine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | (R)-1-(5-hydroxyhexyl)-8-(2-chloroethylamino)-3-methylxanthine | HCID 69154242 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | (R)-1-(5-acetoxyhexyl)-8-(2-chloroethylamino)-3-methylxanthine | HCID 69154552 | 89.1% |
Reaction Steps
To a stirring mixture of (R)-8-(2-chloroethylamino)-1-(5-hydroxyhexyl)-3-methylxanthine (2.2 g, 6.4 mmol), triethylamine (1.94 g, 19.2 mmol) and 4-dimethylaminopyridine (0.39 g, 3.2 mmol) in chloroform (50 ml) at 0-5° C. was added acetic anhydride (1.30 g, 12.8 mmol). The mixture was warmed to room temperature, stirred overnight, and concentrated under reduced pressure. The residue was purified by column chromatography eluting with ethylacetate-methanol (7:1) to provide (R)-1-(5-acetoxyhexyl)-8-(2-chloroethylamino)-3-methylxanthine (2.2 g, 89% yield) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07247630B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-277c249a883c415d872db9d741c0a732 |
| Source note | uspto-grants-2007_07 |