HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 20301784, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 20301725 | HCID 20301725 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 20301784 | HCID 20301784 | — |
Reaction Steps
28.6 g of 8-chloro-4-methyl-1-phenyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one in 100 ml dimethylformamide is stirred with 18 g methyl iodide and 14 g anhydrous potassium carbonate for 2 hours on a boiling water bath. The reaction mixture is poured into 500 ml water and extracted with ether several times. The ethereal extracts are washed with water and dried over sodium sulfate. Upon distilling off the solvent, the crystalline residue is recrystallized from acetic acid ethyl ester. The yield is 24.5 g having an m.p.=113° C.-114° C. (82% of the theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04239684 |
| Source dataset | uspto-grants-1980_12 |
| ORD ID | ord-60f8b8d4815f4d57a0008033911bd02c |
| Source note | uspto-grants-1980_12 |