HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 9904109, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | HCID 9900259 | HCID 9900259 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9904109 | HCID 9904109 | — |
Reaction Steps
Sodium tert-butoxide (10 mg, 0.11 mmol, 1.0 equiv) and iodomethane (13 μL, 0.22 mmol, 2.0 equiv) were added sequentially to a suspension of the product from Example 3 (30 mg, 0.11 mmol, 1 equiv) in THF (10 mL) at 23° C. The reaction mixture was stirred for 20 hours. Additional sodium tert-butoxide (20 mg, 0.22 mmol, 2.0 equiv) and iodomethane (26 μL, 0.44 mmol, 4.0 equiv) were added in 2 equal portions over 1 hour, and then the reaction mixture was allowed to stir an additional 1 hour. Water (5 mL) was added, and the resulting mixture was concentrated to a volume of 2 mL. The mixture was purified by reverse phase HPLC to afford the titled compound as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313138B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-0680d389db804a07988a6919fc32fa68 |
| Source note | uspto-grants-2001_11 |