HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thionyl Chloride → 2-Acetylamino-4-chloromethylpyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | 2-Acetylamino-4-hydroxymethylpyrimidine | HCID 67160710 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Acetylamino-4-chloromethylpyrimidine | HCID 45119260 | 18% |
Reaction Steps
Thionyl chloride (0.18 mL, 2.4 mmol) was added to a suspension of 2-acetylamino-4-hydroxymethylpyrimidine (290 mg, 1.7 mmol, Reference Compound No. 4-3) in anhydrous methylene chloride (10 mL) at room temperature, and the mixture was stirred for 30 minutes. The solvent was evaporated under reduced pressure, then water (50 mL) and ethyl acetate (100 mL) were added thereto and the mixture was separated into the organic layer and the aqueous layer, and the aqueous layer was extracted twice with ethyl acetate (50 mL). The whole organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give 68 mg of the title Reference Compound as a yellow solid (Yield: 18%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07906511B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-0c7ee0cb596244ab94896d40d2c58aa8 |
| Source note | uspto-grants-2011_03 |