HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetyl chloride → N-(4,6-dimethoxypyrimidin-5-yl)chloroacetamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | 4,6-Dimethoxypyrimidin-5-amine | HCID 2817979 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-(4,6-dimethoxypyrimidin-5-yl)chloroacetamide | HCID 15585336 | — |
Reaction Steps
A sulphonation flask is charged with 310 g 5-amino-4,6-dimethoxypyrimidin and 3500 ml dry CH2Cl2. To this mixture is added, within 15 minutes, a solution of 248.6 g chloroacetyl chloride in 400 ml dry CH2Cl2. The reaction is exothermic, the temperature rises from 14° to 32° and a suspension is formed. The reaction mixture is heated under reflux for 2 hours, then cooled to ambient temperature and evaporated till dryness. The solid residue is suspended in 3 l ice water, the suspension adjusted at pH 7-8 with diluted NaOH, cooled to 5° and sucked-off. The precipitate is washed twice with 500 ml ice water and then dried in vacuum at 60° to give the title compound, m.p. 193°-195°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04657579 |
| Source dataset | uspto-grants-1987_04 |
| ORD ID | ord-a82ed227ee60475cb45998e02ccc696a |
| Source note | uspto-grants-1987_04 |