HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diphosgene → HCID 57864416, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diphosgene | HCID 10426 | — |
| Reactant | HCID 57864411 | HCID 57864411 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 57864416 | HCID 57864416 | 23% |
Reaction Steps
A solution of 566.6 mg (2.86 mmol) of trichloromethyl chloroformate in 2.5 ml of dry dioxane is mixed with 1.0 g of 4-[3-((E)-2-{2-[(4-tert-butylbenzyl)oxy]phenyl}vinyl)-7-cyanoheptyl]-benzohydrazide from Example 97A (crude product) in 7.5 ml of dioxane and heated to reflux for 3 hours. The mixture is then directly taken up on silica gel, concentrated to dryness and purified by flash chromatography (mobile phase: dichloromethane/methanol 5:1). 236 mg (0.429 mmol, 23% yield based on two stages) of a solid are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07998988B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-1605b0eba58e4eeeb77ebc535eb9a078 |
| Source note | uspto-grants-2011_08 |