HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 15678855, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | m-Phenylenediisothiocyanate | HCID 18404 | — |
| Reactant | HCID 15678852 | HCID 15678852 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 15678855 | HCID 15678855 | 51.2% |
Reaction Steps
5,11-Dihydro-11-[(4-[10-aminodecyl]-1-piperazinyl)acetyl]-6H-pyrido[2,3-b][1,4]-benzodiazepine-6-one (2.8 mg, 5.7 μmol) was dissolved in 0.2 mL DMF and treated with 1,3-phenylenediisothiocyanate (6 mg, 31 μmol). After 0.5 h, ethyl acetate (1 mL) and petroleum ether (3 mL) were added, and the cloudy mixture was stored at 4° C. overnight. The supernatant was decanted from the oily residue. The residue solidified upon trituration with dry ether to give 2.0 mg (51% yield) of pure product (Rf =0.35, silica, chloroform:methanol:acetic acid, 85:10:5, by volume). FAB-MS spectrum showed a parent ion peak at 685 m/z (m+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05324832 |
| Source dataset | uspto-grants-1994_06 |
| ORD ID | ord-e44c58059c7e41e2aa3f2cb3c92b86b9 |
| Source note | uspto-grants-1994_06 |