HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 123642442, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Di-tert-butyl dicarbonate | HCID 90495 | — |
| Reactant | HCID 86812154 | HCID 86812154 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 123642442 | HCID 123642442 | 86.8% |
Reaction Steps
A mixture of 4-(aminomethyl)phthalazin-1(2H)-one hydrochloride hydrate (0.300 g, 1.31 mmol), BOC2O (0.314 g, 1.44 mmol), and triethylamine (0.46 mL, 3.3 mmol) in DCM (4.5 mL) was stirred for 2 hours, diluted with EtOAc, washed with saturated NaHCO3 and brine, dried (Na2SO4), filtered, and chromatographed (70% EtOAc/hexanes) to give 313 mg of the title compound as a white solid: 1H NMR (300 MHz, DMSO-d6) δ 12.62-12.50 (m, 1H), 8.30-8.22 (m, 1H), 8.01 (s, 1H), 7.92 (dd, J=11.0, 4.1, 1H), 7.89-7.80 (m, 1H), 7.41-7.26 (m, 1H), 4.44 (d, J=5.8, 2H), 1.39 (s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08859549B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-9f15c02941ff4f28a0921f6f2e3de59a |
| Source note | uspto-grants-2014_10 |