Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | N-Boc-5-Hydroxyindoline | HCID 10657398 | — |
| Edukt | Methanesulfonic acid 4-tert-butyl-cyclohexyl ester | HCID 11128255 | — |
| Lösungsmittel | tert-Butanol | HCID 6386 | — |
| Lösungsmittel | Methyl Ethyl Ketone | HCID 6569 | — |
| Produkt | HCID 178451617 | HCID 178451617 | 100% |
Reaktionsschritte
A mixture of 5-hydroxy-2,3-dihydro-indole-1-carboxylic acid tert-butyl ester (0.6 g, 2.6 mmol) in tert-butyl alcohol (8 ml) and 2-butanone (4 mL) was added cesium carbonate (2.5 g, 7.7 mmol) followed by methanesulfonic acid 4-tert-butyl-cyclohexyl ester (1.9 g, 7.7 mmol). The mixture was heated in a sealed vial at 100° C. over night to form precipitate. The mixture was treated with dichloromethane and the precipitate was filtered off and the solvent was concentrated. The residue was purified with a silica gel column eluted with ethyl acetate in hexanes from 0 to 30% to give precipitate (0.96 g, yield: 100%). ESI-MS: 373.30 (M)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US09186367B2 |
|---|
| Quelldatensatz | uspto-grants-2015_11 |
|---|
| ORD ID | ord-2c210c25e06a49b29d6831d82278e2e9 |
|---|
| Quellennotiz | uspto-grants-2015_11 |
|---|