HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → (5R)-4-chloro-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-7-yl acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | (R)-4-chloro-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidine 1-oxide | HCID 58111337 | — |
| Product | (5R)-4-chloro-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-7-yl acetate | HCID 58111335 | 44.4% |
Reaction Steps
A solution of the (R)-4-chloro-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidine 1-oxide (5.5 g, 29.8 mmol) in Ac2O (40.5 mL, 429 mmol) was heated to 110° C. for 3 hours. After cooling, the acetic anhydride was evaporated, and the resulting residue was taken up in DCM. This solution was added to a stirring cold solution of saturated NaHCO3. The layers were extracted with DCM, dried MgSO4, filtered, and concentrated. The crude oil was chromatographed (Biotage) eluting with 20% EtOAc/hexane, to provide (5R)-4-chloro-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-7-yl acetate (3.0 g, 44.4%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08895566B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-ea7061b7b55346b19bb582a9d30d86e0 |
| Source note | uspto-grants-2014_11 |