Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 4-Bromo-2-(2-bromo-ethyl)-benzenesulfonyl chloride | HCID 58016189 | — |
| Edukt | HCID 137328873 | HCID 137328873 | — |
| Lösungsmittel | 1,1-Dichloroethane | HCID 6365 | — |
| Produkt | HCID 178455419 | HCID 178455419 | 53,4% |
Reaktionsschritte
The mixture of 5-[3-Amino-2-(tert-butyl-dimethyl-silanyloxymethyl)-phenyl]-1-methyl-3-[5-(morpholine-4-carbonyl)-pyridin-2-ylamino]-1H-pyridin-2-one (0.2 g, 0.36 mmol), 4-bromo-2-(2-bromo-ethyl)-benzenesulfonyl chloride (0.4 g, 1.08 mmol) and DIPEA (1 mL) in dichloroethane (10 mL) was microwaved at 120° C. for 30 min, then added 4-bromo-2-(2-bromo-ethyl)-benzenesulfonyl chloride (0.4 g, 1.08 mmol) and DIPEA (1 mL) and microwaved at 120° C. for 30 min. After repeating this process three times, the mixture was concentrated to afford a dark residue. Purification by silica gel chromatography (methylene chloride/acetone) afforded 0.15 g of 5-[3-(6-Bromo-1,1-dioxo-3,4-dihydro-1H-1lambda*6*-benzo[e][1,2]thiazin-2-yl)-2-(tert-butyl-dimethyl-silanyloxymethyl)-phenyl]-3-[5-(morpholine-4-carbonyl)-pyridin-2-ylamino]-1H-pyridin-2-one as a pale solid MS (ESI) 796.2 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07902194B2 |
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| Quelldatensatz | uspto-grants-2011_03 |
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| ORD ID | ord-e3b8f0dc12264f1fa9c6244cdae7b8ee |
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| Quellennotiz | uspto-grants-2011_03 |
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