Reaktionsgleichung
[Br:1][C:2]1[CH:7]=[CH:6][C:5](/[N:8]=[C:9](/[O:16][CH2:17][CH3:18])\[CH2:10][C:11]([O:13]CC)=O)=[CH:4][C:3]=1[O:19][CH3:20]>C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1>[Br:1][C:2]1[CH:7]=[C:6]2[C:5](=[CH:4][C:3]=1[O:19][CH3:20])[N:8]=[C:9]([O:16][CH2:17][CH3:18])[CH:10]=[C:11]2[OH:13]Komponenten
3
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 250 °C
Versuchsvorschrift
To a stirred solution of DOWTHERM (300 mL) at 250° C. was added a solution of the product of Step 2 (30.0 g, 87 mmol) in DOWTHERM (30 mL). The resulting solution was stirred at 250° C. for 5 minutes, cooled to RT and filtered. The resulting cake was washed with hexane (3×50 mL), then dried to give the title product. 1H NMR (400 MHz, CD3OD) δ 8.25 (s, 1H); 6.92 (s, 1H); 5.80 (s, 1H); 4.27 (q, J=7.1 Hz, 2H); 3.97 (s, 3H); 1.46 (t, J=7.0 Hz, 3H) ppm. LRMS (ESI) m/z 298.0 [(M+H)+; calcd for C12H13BrNO3: 298.0].
Aufarbeitung
- temperaturecooled to RT
- filtrationfiltered
- washThe resulting cake was washed with hexane (3×50 mL)
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-14c7306fa87044b0b756d602788f85e3
- Quelldatensatz
- uspto-grants-2013_02
- Patentnummer
- US08377874B2
Verknüpfte Notizen
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