HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetyl chloride → HCID 86722014, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | HCID 22180015 | HCID 22180015 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 86722014 | HCID 86722014 | 61% |
Reaction Steps
To a solution of 1-amino-3-chloro-1H-pyrrole-2-carboxylic acid (12.51 g, 55% purity, 0.04 mol) in 500 mL of glacial acetic acid were added under argon 17 mL of chloroacetyl chloride (0.21 mol) and the mixture was stirred at room temperature during 1.5 hours. Afterwards, the reaction mixture was poured into ice-water and extracted with ethyl acetate (2×400 mL). The organic layers were washed with water and brine, dried (MgSO4) and concentrated in vacuum giving a dark oil that was crystallized from a 1/1 diethyl ether/petroleum ether mixture. Filtration of the solid obtained afforded 7.28 g of a white solid corresponding to the title compound (61% yield, 85% purity). This solid was used in the next step without further purifications.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09340547B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-22b73261b6b840b091a3493a97701130 |
| Source note | uspto-grants-2016_05 |