HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetyl chloride → HCID 54401423, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Water ethylacetate | HCID 22728543 | — |
| Reactant | HCID 54324264 | HCID 54324264 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54401423 | HCID 54401423 | — |
Reaction Steps
To a solution of 4-(3-amino-4-chloro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (500 mg) and N,N-diisopropylethylamine (0.8 ml) in tetrahydrofuran (20 ml) cooled to 0° C. was added 2-chloroacetyl chloride (0.2 ml). After 2 hrs, the reaction was poured into ethyl acetate/water. The organic layer was separated, washed with water, aqueous NaHCO3 and brine, dried (MgSO4) and concentrated. Purification of the residue by silica gel chromatography (eluting ethyl acetate/iso-hexane (1:3 to 1:2) gave the sub-title product (0.5 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06555541B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-edc834d5531349cd881a3e2648b56bf0 |
| Source note | uspto-grants-2003_04 |