HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl carbazate → N1-(tert-butoxycarbonyl)-N2-(4-biphenylylmethyl)hydrazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl carbazate | HCID 70091 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1,1'-Biphenyl, 4-(bromomethyl)- | HCID 257716 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | N1-(tert-butoxycarbonyl)-N2-(4-biphenylylmethyl)hydrazine | HCID 10637828 | 70.3% |
Reaction Steps
4-(Bromomethyl)biphenyl (2.0 g, 8.1 mmol, 1.0 eq.) and DIPEA (1.4 mL, 1.0 eq.) were dissolved in DMF (40.0 mL). t-Butyl carbazate (2.1 g, 16.2 mmol, 2.0 eq.) was added and the mixture was stirred at room temperature overnight. The mixture was partially concentrated, and the residue was partitioned between EtOAc and a saturated aqueous NaHCO3 solution. The EtOAc layer was then dried over Na2SO4 and concentrated. The crude product was purified by flash chromatography (0-60% EtOAc/hexanes with 0.5% DIPEA) to yield compound 1, N′-biphenyl-4-ylmethyl-hydrazinecarboxylic acid t-butyl ester (1.7 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08563512B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-c5a870ffd848454c9efcb41a44c92624 |
| Source note | uspto-grants-2013_10 |