HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 17961979, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Fluoride | HCID 5235 | — |
| Reactant | HCID 17961962 | HCID 17961962 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 17961979 | HCID 17961979 | 86.2% |
Reaction Steps
To a mixture of lithium aluminum hydride (32.6 g) in tetrahydrofuran (1.3 L) was added (2E)-3-[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]-2-propenonitrile (101.6 g) under ice-cooling. The mixture was refluxed for 4 hours. After cooling on an ice bath, sodium fluoride (100 g) and water (100 ml) were added to the reaction mixture. The insoluble materials were removed by filtration. The filtrate was concentrated in vacuo to give 4-(3-aminopropyl)-1-methyl-5-tritylamino-1H-pyrazole (88.9 g). 1H-NMR(DMSO-d6) δ1.00–1.22 (2H, m), 1.70–1.90 (2H, m), 2.15–2.35 (2H, m), 2,74 (3H, s), 5.70 (1H, s), 6.97 (1H, s), 7.10–7.38 (15H, m)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07179801B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-304d96c3a6ab40a6b222b85273b50059 |
| Source note | uspto-grants-2007_02 |