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Cesium carbonate → 4-[7-(2-chloro-5-methoxy-phenyl)-5-methyl-benzo[1,2,4]triazin-3-ylamino]-N-methyl-N-(2-pyrrolidin-1-yl-ethyl)-benzenesulfonamide

HRID 449196
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 449196
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:20]=[C:19]([CH3:21])[C:13]2[N:14]=[C:15]([NH2:18])[N:16]=[N:17][C:12]=2[CH:11]=1.Br[C:23]1[CH:28]=[CH:27][C:26]([S:29]([N:32]([CH3:40])[CH2:33][CH2:34][N:35]2[CH2:39][CH2:38][CH2:37][CH2:36]2)(=[O:31])=[O:30])=[CH:25][CH:24]=1.C([O-])([O-])=O.[Cs+].[Cs+].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:20]=[C:19]([CH3:21])[C:13]2[N:14]=[C:15]([NH:18][C:23]3[CH:28]=[CH:27][C:26]([S:29]([N:32]([CH3:40])[CH2:33][CH2:34][N:35]4[CH2:36][CH2:37][CH2:38][CH2:39]4)(=[O:31])=[O:30])=[CH:25][CH:24]=3)[N:16]=[N:17][C:12]=2[CH:11]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 248227537-(2-Chloro-5-methoxyphenyl)-5-methylbenzo[e][1,2,4]triazin-3-amineHCID 598376194-bromo-N-methyl-N-(2-pyrrolidin-1-yl-ethyl)-benzenesulfonamide

Produkt 1

HCID 59837674
4-[7-(2-chloro-5-methoxy-phenyl)-5-methyl-benzo[1,2,4]triazin-3-ylamino]-N-methyl-N-(2-pyrrolidin-1-yl-ethyl)-benzenesulfonamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysatorHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

7-(2-chloro-5-methoxy-phenyl)-5-methyl-benzo[1,2,4]triazin-3-ylamine (0.33 mmol, 1.0 equiv), 4-bromo-N-methyl-N-(2-pyrrolidin-1-yl-ethyl)-benzenesulfonamide (0.5 mmol, 1.5 equiv), Cs2CO3 (0.99 mmol, 3.0 equiv), Pd2(dba)3 (0.033 mmol, 0.10 equiv.), and Xantphos (0.066 mmol, 0.2 equiv) were dissolved in 10 mL dioxane and refluxed at 100° C. under an argon atmosphere for 18 h. The reaction was cooled to room temperature and filtered. The filtrate was dissolved in EtOAc and washed with saturated NaHCO3 and brine, and the organic phase was dried (Na2SO4). The organics were concentrated under reduced pressure to afford residue that was purified by reverse phase HPLC using a 10-50-75 gradient over 30 minutes, and again concentrated under reduced pressure to afford 4-[7-(2-chloro-5-methoxy-phenyl)-5-methyl-benzo[1,2,4]triazin-3-ylamino]-N-methyl-N-(2-pyrrolidin-1-yl-ethyl)-benzenesulfonamide, as a tan residue (168 mg, 90% yield). Rf=0.50 (9:1 DCM/MeOH) MS (ES+) m/z=567. LC retention time 2.82 min.

Aufarbeitung

  1. temperatureThe reaction was cooled to room temperature
  2. filtrationfiltered
  3. dissolutionThe filtrate was dissolved in EtOAc
  4. washwashed with saturated NaHCO3 and brine
  5. dry with materialthe organic phase was dried (Na2SO4)
  6. concentrationThe organics were concentrated under reduced pressure
  7. customto afford residue
  8. customthat was purified by reverse phase HPLC
  9. customover 30 minutes
  10. concentrationagain concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-2a20b9a6ccd64876bc2849bf62127a00
Quelldatensatz
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08481536B2

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