HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 59639635, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 10113314 | HCID 10113314 | — |
| Product | HCID 59639635 | HCID 59639635 | — |
Reaction Steps
The product of Example 59 (200 mg, 0.47 mmol) was placed in EtOH (10 mL) and the mixture stirred under Ar. Approximately 2 mL of the ethanol was distilled off to dry the mixture. When the mixture was cooled to 23°, some of the starting material sulfone crystallized out. NaH (11.5 mg, 0.46 mmol) was added. The reaction did not go to completion, so additional NaH (4 mg, 0.16 mmol) was added. The solvent was removed in vacuo, and the residue was flash chromatographed on silica gel eluted with 60-100% CH2Cl2/hexane. Recrystallization from CH2Cl2/hexane gave the title compound as a white crystalline solid. mp 137-139°, LC MS m/z=394(MH+) Retention time=2.32 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08058282B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-d100dd75991a48c78df0d2213f37af35 |
| Source note | uspto-grants-2011_11 |