HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon Tetrachloride → HCID 90273397, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon Tetrachloride | HCID 5943 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | HCID 90273127 | HCID 90273127 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 90273397 | HCID 90273397 | — |
Reaction Steps
To a solution of 4-[N′-(2-amino-5-bromo-pyridine-3-carbonyl)-hydrazinocarbonyl]-piperidine-1-carboxylic acid tert-butyl ester (1.3 g, 2.939 mmol) in ACN (50 mL) were added DBU (1.68 g, 11.035 mmol), PPh3 (1.95 g, 7.434 mmol) and CCl4 (4 mL, 41.558 mmol) at RT. The reaction mixture was stirred for 18 h at RT. The reaction mixture was poured into ice-water (30 mL), extracted with ethyl acetate (3×50 mL), organic layer was washed with brine dried over anhydrous sodium sulphate concentrated under reduced pressure. Crude compound was purified by column chromatography using 100-200 mesh silica gel. The column was eluted with 40% EtOAc in petroleum ether to afford the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09321748B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-d741a3f18d0642ef8a891a4567b61db1 |
| Source note | uspto-grants-2016_04 |