Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | Tritylamine | HCID 138598 | — |
| Edukt | 1,2-Bis(bromomethyl)-4-iodobenzene | HCID 66726722 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 5-Iodo-2-tritylisoindoline | HCID 66726248 | 48% |
Reaktionsschritte
A mixture of the product of Step B (0.34 g; 0.87 mmol) hydrochloride salt of tritylamine (0.22 g; 0.87 mmol) and N,N-diisopropylethylamine (DIPEA) (0.49 ml; 2.8 mmol) in anhydrous DMF (3 ml) was stirred for 2 h at 60° C. under N2. After removing the solvent in vacuo, the residue was diluted to 15 ml with ethyl acetate (EtOAc) and washed with, H2O, brine and dried over anhydrous MgSO4 and filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was purified by FCC (SiO2; hexane/EtOAc, 8:2) to give pure title compound (0.2 g; 48%) as colourless heavy syrup. 1H-NMR (CDCl3) 3.86 (s, 2H); 3.87 (s, 2H); 6.81-7.57 (m, 18H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09181182B2 |
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| Quelldatensatz | uspto-grants-2015_11 |
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| ORD ID | ord-2b25a432ae864e688dac041a97b72a02 |
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| Quellennotiz | uspto-grants-2015_11 |
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