HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 13606573, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 20204018 | HCID 20204018 | — |
| Reactant | Acetic Acid Mixture with Hydrobromic Acid | HCID 21893785 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 13606573 | HCID 13606573 | 79.3% |
Reaction Steps
1-(p-(N-Benzylcarbonylamino)benzyl)-3-(1,3-dithiol-2-ylidene)-2,4-dioxopiperidine (100 mg) is dissolved in acetic acid (2 ml), and a 25% HBr-acetic acid solution (0.5 ml) is added thereto. The mixture is stirred at room temperature for 40 minutes, and then at 40°-50° C. for one hour. After cooling the mixture, ether is added to the mixture. The precipitated crystals are collected by filtration, and recrystallized from a mixture of methanol and ether to give 1-(p-aminobenzyl)-3-(1,3-dithiol-2-ylidene)-2,4-dioxopiperidine hydrobromide (70 mg, 79.3%) as pale yellow needles, m.p. 210°-214° C. (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04663319 |
| Source dataset | uspto-grants-1987_05 |
| ORD ID | ord-102a95fff05a4530a7126131c04dad02 |
| Source note | uspto-grants-1987_05 |