HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 5273039, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 9845603 | HCID 9845603 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 5273039 | HCID 5273039 | — |
Reaction Steps
The product of Example 12 (627 mg, 1.46 mmol) was added to a freshly prepared solution of sodium methoxide in methanol (1.5 equivalents sodium in 5 mL methanol) in dry dimethylformamide (3-5 mL) and the mixture was stirred at room temperature for 15-30 minutes. The reaction mixture was diluted with water and extracted with ethyl acetate (3x). The combined organic extracts were washed with water, brine, dried (MgSO4) and concentrated in vacuo. The crude residue (0.64 g) was purified by chromatography (Silica Gel 60, first with 2% methanol in methylene chloride followed by 5% ethyl acetate in methylene chloride) to give pure title compound (308 rag) as a colorless oil which crystallized from methanol, mp 64.5°-65.5° C. (white solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05464848 |
| Source dataset | uspto-grants-1995_11 |
| ORD ID | ord-749f61de508e4b7a98fe5e91808e00c1 |
| Source note | uspto-grants-1995_11 |