HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric acid magnesium salt (1:1) → HCID 88932543, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | tert-Butyl carbazate | HCID 70091 | — |
| Reactant | 2-((Tert-butyldimethylsilyl)oxy)acetaldehyde | HCID 4187788 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 88932543 | HCID 88932543 | 94% |
Reaction Steps
A mixture of tert-butyl hydrazinecarboxylate (2.5 g, 19 mmol), MgSO4 (11.4 g, 95.0 mmol), and 2-(tert-butyldimethylsilyloxy)acetaldehyde (9.9 g, 57 mmol) in DCM (100 mL) was heated to reflux overnight. The solid was filtered off and the filtrate was concentrated. The residue was purified by silica gel chromatography eluting with EtOAc/petroleum ether (1:5) to give (E)-tert-butyl 2-(2-(tert-butyldimethylsilyloxy)ethylidene)hydrazinecarboxylate (5.1 g, 94% yield) as colorless oil. LCMS (ESI) m/z: 233.3 [M-56+H+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09090628B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-a90f56458e7e4123a2e0867757b578cd |
| Source note | uspto-grants-2015_07 |