HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylcarbamoyl Chloride → HCID 15136679, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Reactant | 4,4-Dimethyl-1-phenyl-3-pyrazolidone | HCID 75861 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 15136679 | HCID 15136679 | 73% |
Reaction Steps
To a solution of 4,4-dimethyl-1-phenyl-3-pyrazolidinone (1.90 g) in a mixture of 25 mL pyridine and 4 mL triethylamine at 0° C. is added N,N-dimethylcarbamoyl chloride (1.37 mL). The reaction mixture is stirred at room temperature for 16 hours. The reaction mixture is diluted with methylene chloride (100 mL) and washed with 10% aqueous hydrochloric acid (200 mL). The organic layer is dried (MgSO4), filtered and evaporated. Chromatography on silica gel gave a light yellow solid. Recrystallization from ethanol gave 1.80 g (73%) of pale yellow crystals. (MP-99°-100° C.; Analysis: C-64.26%, H-7.19%, N-16.04%; H1NMR-δ 7.6-2H,t; δ 7.35-2H,d; δ 7.15-2H,t; δ 4.1-2H,s; δ 3.4-3H,s; δ 3.3-3H,s; δ 1.7-6H,s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04999368 |
| Source dataset | uspto-grants-1991_03 |
| ORD ID | ord-7e2066bb775a46348bf37b877e75e3fe |
| Source note | uspto-grants-1991_03 |