HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 19972853, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Methyl-2-butenoic acid | HCID 10931 | — |
| Reactant | Diethylphosphorylcyanide | HCID 13586794 | — |
| Reactant | 2-aminomethyl-5-[pyridazin-3(2H)-on-6-yl]indane hydrobromide | HCID 21476291 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19972853 | HCID 19972853 | 79.8% |
Reaction Steps
Under ice cooling, 1.71 g of diethylphosphoryl cyanide was added to 80 ml of a suspension containing 3.06 g of 2-aminomethyl-5-[pyridazin-3(2H)-on-6-yl]indane·hydrobromide and 1.15 g of 3-methylcrotonic acid suspended in dimethylformamide, and then 20 ml of a solution containing 2.89 g of triethylamine dissolved in dimethylformamide was added dropwise to the mixture. The resulting mixture was stirred at the same temperature for 2.5 hours. The reaction mixture was poured into ice water, and crystals precipitated were collected by filtration. The crystals obtained were washed with water, dried and then recrystallized from ethyl acetate-methanol to obtain 2.45 g of 2-[(3-methylcrotonoyl)amino]methyl-5-[pyridazin-3(2H)-on-6-yl]indane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05605901 |
| Source dataset | uspto-grants-1997_02 |
| ORD ID | ord-aef722d888424d109e975a5f148e1212 |
| Source note | uspto-grants-1997_02 |