HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane → HCID 136026810, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Acetamidine monohydrochloride | HCID 67170 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 57460183 | HCID 57460183 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 136026810 | HCID 136026810 | 86% |
Reaction Steps
To a solution of acetamidine hydrochloride (3.4 g) in methanol (30 mL) was added sodium methoxide (28% methanol solution, 10.3 g) at 0° C., a solution of methyl 2-[(2′-cyanobiphenyl-4-yl)methyl]-4-methoxy-3-oxobutanoate in methanol (60 mL)-1,4-dioxane (20 mL) was added, and the mixture was stirred at room temperature for 16 hr. The reaction mixture was concentrated, and water (50 mL) and 50% aqueous acetic acid solution were added to the residue and adjusted to pH 5. The obtained crystallized product was collected by filtration and washed with water to give the title compound as colorless crystals (5.27 g, 86%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07998968B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-434ad438fb354b81861119a5c81e924a |
| Source note | uspto-grants-2011_08 |