HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 117770681, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 4,6-Dichloropyrimidine | HCID 70943 | — |
| Reactant | 1-(2-Hydroxyethyl)-2-pyrrolidinone | HCID 76980 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 117770681 | HCID 117770681 | — |
Reaction Steps
To a solution of 4,6-dichloropyrimidine (600 mg) and 1-(2-hydroxyethyl)-2-pyrrolidinone (0.728 mL) in N,N-dimethylformamide (2 mL) was added sodium hydride (60% oil, 209 mg) under ice-cooling, and the mixture was stirred for 30 min. The reaction mixture was poured into saturated aqueous ammonium chloride solution (10 mL), water (5 mL) was added thereto, and the mixture was extracted with ethyl acetate. The organic layer was washed with, water (10 mL, threetimes) and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained pale-yellow oil was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (634 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09085578B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-cee829f39729407f9f3d2ba55cd4c380 |
| Source note | uspto-grants-2015_07 |