HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide dimethyl acetal → HCID 67435184, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| Reactant | 1-(2-Chlorophenyl)butane-1,3-dione | HCID 14987993 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 67435184 | HCID 67435184 | 51% |
Reaction Steps
A mixture of crude 1-(2-chlorophenyl)butane-1,3-dione from the previous step and 1,1-dimethoxy-N,N-dimethylmethanamine (2.042 g, 17.14 mmol) in toluene (20 mL) was heated to reflux for 2 h and concentrated. Silica gel chromatography, using 70 to 100% ethyl acetate in hexanes gradient, gave 1-(2-chlorophenyl)-2-((dimethylamino)methylene)butane-1,3-dione as a red, viscous oil (2.20 g, 51% yield for 2 steps). MS (ES+) m/z: 252 (M+H); HPLC retention time: 2.51 min (Analytical HPLC Method D).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08034940B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-c1a3458a245b47feb21a7ba557415bb9 |
| Source note | uspto-grants-2011_10 |