HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trichloroacetyl chloride → HCID 21190140, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trichloroacetyl chloride | HCID 6420 | — |
| Reactant | HCID 21190090 | HCID 21190090 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21190140 | HCID 21190140 | 47.9% |
Reaction Steps
To a solution of 7.69 g (18.56 mmol) of 5-[N-tert-butoxycarbonyl-N-(4-trifluoroacetamidobutan-1-yl)amino methyl]imidazo[1,2-a]pyridine and 10.20 g (83.52 mmol) of 4-(N,N-dimethylamino)pyridine in 100 ml of THF was added 6.21 ml (55.67 mmol) of trichloroacetyl chloride. The reaction mixture was heated for 16 hours under reflux. The reaction mixture was poured into ice-water, and extracted with 100 ml of ethyl acetate. The organic layer was washed with 150 ml of a saturated aqueous saline solution, dried over magnesium sulfate, and distilled off the solvent under reduced pressure. The residue was purified by silica gel column chromatography (eluent; chloroform) to afford 4.98 g of the desired compound (48.0%, a pale yellow amorphous).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05958942 |
| Source dataset | uspto-grants-1999_09 |
| ORD ID | ord-1e25b9e1881344f68f451991b7634520 |
| Source note | uspto-grants-1999_09 |