HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 53751272, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Acetic-formic anhydride | HCID 75269 | — |
| Reactant | 1-[(4-Chlorophenyl)methyl]-2-(nitromethylidene)hexahydropyrimidine | HCID 67844408 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 53751272 | HCID 53751272 | — |
Reaction Steps
1-(4-Chlorobenzyl)-2-nitromethylene-hexahydropyrimidine (3 g) was added to a stirred suspension of sodium hydride (0.54 g) in dry dimethylformamide (150 ml) at room temperature under nitrogen and the stirring was continued overnight. Formic acetic anhydride (100% excess) was then added dropwise to the stirred suspension at 0°. The reaction mixture was then stirred for 1 hour. It was then poured onto water and extracted with dichloromethane (2×200 ml). The combined organic layers were dried (sodium sulphate) and the solvent removed in vacuo, to leave a solid. The solid was triturated with chloroform (5 ml) and was then filtered off, washed with chloroform (5 ml) and dried to afford the title compound (1.2 g), m.pt. 131°-133° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04758570 |
| Source dataset | uspto-grants-1988_07 |
| ORD ID | ord-952c15934386463ca715b51f4663c9b1 |
| Source note | uspto-grants-1988_07 |