HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetamidine monohydrochloride → HCID 178467223, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetamidine monohydrochloride | HCID 67170 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 3-Chloro-4,4-dimethoxybutan-2-one | HCID 15587945 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178467223 | HCID 178467223 | 75.2% |
Reaction Steps
A mixture of 1.66 g (10 mmole) 2-chloro-1,1-dimethoxy-3-butanone, 1.43 g (15 mmole) acetamidine hydrochloride and 2.05 g (25 mmole) sodium acetate in 50 ml dioxane is heated at reflux for 24 hours. The dioxane is evaporated in vacuo and the residual oil is flash chromatographed on silica gel (40:60 ethyl acetate/hexane, 40 mm) to obtain three fractions. The third fraction, a white solid (1.121 g) was rechromatographed (40 mm, acetone) to afford 933 mg (75.1%) of product as white solid which is pure as judged by its NMR spectrum in CDCl3 and by TLC on silica gel (one spot, 1:9 methanol/chloroform).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04482723 |
| Source dataset | uspto-grants-1984_11 |
| ORD ID | ord-a3a1abfa6cbe4a99a8e3c91926f0eb40 |
| Source note | uspto-grants-1984_11 |