Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 21834554 | HCID 21834554 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67761997 | HCID 67761997 | 98.1% |
Reaction Steps
Sodium hydride (80% in mineral oil, 1.53 g, 51 mmol) was stirred in dry DMF (30 ml) as 4'-(2-fluorophenyl)-4'-(hydroxymethyl)spiro[[1,3]-dioxolane-2,1 '-cyclohexane] (D22, 5.44 g, 20 mmol) was added in dry DMF (70 ml). The mixture was stirred under Ar at 110° C. for 6 h, cooled, diluted with ethyl acetate (500 ml), washed with water and brine, dried (Na2SO4) and evaporated to give the title compound (4.83 g, 96%) as a straw-coloured solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05952325 |
|---|
| Source dataset | uspto-grants-1999_09 |
|---|
| ORD ID | ord-9b9ebe471da841e8a0efef3828db5071 |
|---|
| Source note | uspto-grants-1999_09 |
|---|