HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 178462379, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 1-[(1R)-1-chloroethyl]-2-fluorobenzene | HCID 52420308 | — |
| Reactant | HCID 178507962 | HCID 178507962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178462379 | HCID 178462379 | 75% |
Reaction Steps
NaH (60% in oil, 1.05 g, 26.3 mmol) was added in portions followed by NaBH4 (0.099 g, 2.7 mmol) to 6-amino-2-mercaptopyrimidin-4-ol monohydrate (4.23 g, 26.3 mmol) in DMF (40 mL). After 30 minutes, 1-[(1R)-1-chloroethyl]-2-fluorobenzene (5.0 g, 31.5 mmol) in DMF (10 mL) was added and the reaction mixture was stirred for 24 h. The reaction mixture was concentrated and partitioned between water and DCM, the organic phase was dried (MgSO4) and evaporated. The residue was purified by flash column chromatography (a stepwise gradient of 5-10% MeOH in CHCl3) to give the title compound (5.20 g, 75% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08088780B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-24f4336e22864c95b1294f4bc52a3595 |
| Source note | uspto-grants-2012_01 |