HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Thioxo-1,2,3,5,6,7-hexahydro-4h-benzo[6,7]cyclohepta[1,2-d]pyrimidin-4-one → 3,5,6,7-tetrahydro-4H-benzo[6,7]cyclohepta[1,2-d]pyrimidin-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Thioxo-1,2,3,5,6,7-hexahydro-4h-benzo[6,7]cyclohepta[1,2-d]pyrimidin-4-one | HCID 15857126 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 3,5,6,7-tetrahydro-4H-benzo[6,7]cyclohepta[1,2-d]pyrimidin-4-one | HCID 135818706 | — |
Reaction Steps
A solution of Example 118A (170 mg, 0.7 mmol) in methanol (15 mL) was treated with Raney nickel (slurry in H2O, 1 spatula) and refluxed for 16 hours. The mixture was filtered through diatomaceous earth and washed with methanol. The filtrate was concentrated under vacuum to provide the title compound. 1H NMR (CD3OD) δ 2.24 (t, 2H), 2.40 (t, 2H), 2.59 (t, 2H), 7.27-7.34 (m, 1H), 7.36-7.42 (m, 2H), 7.60-7.66 (m, 1H), 8.14-8.18 (m, 1H). MS (M+H)+ m/z 213
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08735411B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-1d07cd99ad4a42b4af7f52173f0c846e |
| Source note | uspto-grants-2014_05 |