HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 88236383, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Butene, 1-bromo-3-methyl- | HCID 70092 | — |
| Reactant | HCID 56626166 | HCID 56626166 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 88236383 | HCID 88236383 | — |
Reaction Steps
50 mg of compound (6) was dissolved in 0.4 ml of dry dimethylformamide under a nitrogen atmosphere and mixed with about 5 mg of sodium hydride under cooling with ice. After 15 minutes, 37.4 ml of 4-bromo-2-methyl2-butene was added, and the reaction solution was stirred under cooling with ice for 50 minutes. The reaction solution was allowed to react at room temperature for another 20 minutes under stirring. Then, the reaction solution was charged onto a silica gel column (Kieselgel 60, Merck, 1.5φ×19 cm) and eluted with n-hexane-ethyl acetate (10:1) to give 34.4 mg of compound (42) as a colorless oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06087390 |
| Source dataset | uspto-grants-2000_07 |
| ORD ID | ord-47ba7640bad44f50aa2c453a1a9610ef |
| Source note | uspto-grants-2000_07 |