HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 20747587, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | 4-Acetylbenzoic Acid | HCID 11470 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 20747587 | HCID 20747587 | 84.2% |
Reaction Steps
A mixture of 4-acetylbenzoic acid (10.0 g, 60.9 mmol), 40% aqueous solution of dimethylamine (8.24 g, 73.1 mmol), EDC (14.0 g, 73.1 mmol), HOBT (11.2 g, 73.1 mmol) and DIEA (21.3 mL, 122 mmol) in CH3CN (150 mL) was stirred at room temperature for 15 h and concentrated. The residue was dissolved in ethyl acetate (600 mL), washed with water (2×80 mL), brine (80 mL), dried (MgSO4) and concentrated to provide 4-acetyl-N,N-dimethylbenzamide (9.80 g, 84%). MS (E+) m/z: 191 (M+H); HPLC retention time: 0.88 min (Analytical HPLC Method F).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08034940B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-b5b603fc6a2a4d2999ec3b807a01474a |
| Source note | uspto-grants-2011_10 |