HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 22729049, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 22728917 | HCID 22728917 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 22729049 | HCID 22729049 | 62.1% |
Reaction Steps
N′-(4-(Methoxymethyloxy)benzo(b)thiophen-2-ylcarbonyl)acetohydrazide (2.4 g) was dissolved in 1,2-dichloroethane (50 ml) and triphenylphosphine (3.2 g) and triethylamine (2 ml) were added. The mixture was stirred under ice-cooling. Diethyl azodicarboxylate (40% toluene solution) (5.2 g) was added and the mixture was stirred at room temperature for 1 hr. The reaction mixture was poured into ice water and extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title product (1.4 g) as pale-yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07196199B2 |
| Source dataset | uspto-grants-2007_03 |
| ORD ID | ord-cb799a39ccba4248a094a324cb8acdc7 |
| Source note | uspto-grants-2007_03 |