HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diphosgene → HCID 57864352, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diphosgene | HCID 10426 | — |
| Reactant | HCID 57864419 | HCID 57864419 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 57864352 | HCID 57864352 | 96.6% |
Reaction Steps
A solution of 185 mg (0.29 mmol, 89% purity) of 4-{(3E)-4-{2-[(4-tert-butylbenzyl)oxy]phenyl}-2-[2-(4-cyanophenyl)ethyl]but-3-en-1-yl}benzohydrazide from Example 103A in 1 ml of dioxane is slowly added dropwise to a solution of 87.3 mg (0.44 mmol) of trichloromethyl chloroformate in 0.5 ml of dioxane. The reaction mixture is stirred under reflux for two hours. After cooling, the mixture is concentrated in vacuo, directly taken up on silica gel and purified by flash chromatography (mobile phase: dichloromethane/methanol/aq. ammonia 10:1:0.1). 166 mg (0.28 mmol, 96% yield) of an oil are isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07998988B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-6d3b56a3072540f39ef38d1046df6ff5 |
| Source note | uspto-grants-2011_08 |