HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 131720207, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3,3-Dimethylbutanoyl chloride | HCID 81514 | — |
| Reactant | HCID 22909965 | HCID 22909965 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131720207 | HCID 131720207 | 75% |
Reaction Steps
A stirred solution of 3-methylamino-1(4-trifluoromethylpyridin-2-yl)pyrrolidin-2-one (0.30 g, prepared as described in Example 7, Step 3, above) in dichloromethane (20 ml) was treated successively with triethylamine (0.13 g) and 3,3-dimethylbutanoyl chloride (0.16 g). After one hour, the mixture was diluted with dichloromethane, washed with water and brine, dried over magnesium sulphate and evaporated under reduced pressure. The residue was chromatographed on silica, using hexane-ethyl acetate (1:1) as eluant, to give Compound 28 (0.31 g, m.p. 47°-53° C.). NMR (CDCl3): δ 1.31(9H,s); 2.31(4H,m+s); 3.09(3H,s); 3.88(1H,m); 4.32(1H,m); 5.22(1H,t); 7.26(1H,dd); 8.52(1H,d); 8.78(1H,s). MS: M+357.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05670656 |
| Source dataset | uspto-grants-1997_09 |
| ORD ID | ord-5638cd4999c541efb9eb0078be916e4c |
| Source note | uspto-grants-1997_09 |