HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butanol → tert-Butyl [2-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)ethyl]carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butanol | HCID 6386 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Phthalimidopropionic acid | HCID 76859 | — |
| Reactant | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | tert-Butyl [2-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)ethyl]carbamate | HCID 11483141 | 72.2% |
Reaction Steps
To a solution of 3-(phthalimido)propionic acid (6.0 g) and triethylamine (2.77 g) in benzene (60 ml) was added diphenylphosphoryl azide (7.53 g), and the mixture was refluxed for 40 minutes. Tert-butanol (4.23 g) was added thereto, and the mixture was refluxed overnight. After cooling, the reaction mixture was washed with saturated sodium bicarbonate solution, water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by flash chromatography (n-hexane-ethyl acetate) and crystallized from diisopropyl ether to give N-(2-tert-butoxycarbonylaminoethyl)phthalimide (5.74 g) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06008229 |
| Source dataset | uspto-grants-1999_12 |
| ORD ID | ord-d3a10745d45f493eb7444858837e16f1 |
| Source note | uspto-grants-1999_12 |