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Cesium carbonate → Tert-butyl cis-2-(3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)-6-(5-methylpyridin-3-ylamino)pyridin-2-ylamino)cyclohexylcarbamate

HRID 1620122
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1620122
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.[NH2:43][C:44]1[N:49]=[C:48]([NH:50][C@H:51]2[CH2:56][CH2:55][CH2:54][CH2:53][C@H:52]2[NH:57][C:58](=[O:64])[O:59][C:60]([CH3:63])([CH3:62])[CH3:61])[C:47]([Cl:65])=[CH:46][C:45]=1[C:66]([NH:68][C:69]([C:72]1[CH:77]=[CH:76][CH:75]=[CH:74][CH:73]=1)([CH3:71])[CH3:70])=[O:67].C(=O)([O-])[O-].[Cs+].[Cs+].Br[C:85]1[CH:86]=[N:87][CH:88]=[C:89]([CH3:91])[CH:90]=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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C(OCC)(=O)C.O.O1CCOCC1>[Cl:65][C:47]1[C:48]([NH:50][C@H:51]2[CH2:56][CH2:55][CH2:54][CH2:53][C@H:52]2[NH:57][C:58](=[O:64])[O:59][C:60]([CH3:63])([CH3:61])[CH3:62])=[N:49][C:44]([NH:43][C:85]2[CH:86]=[N:87][CH:88]=[C:89]([CH3:91])[CH:90]=2)=[C:45]([C:66]([NH:68][C:69]([C:72]2[CH:73]=[CH:74][CH:75]=[CH:76][CH:77]=2)([CH3:70])[CH3:71])=[O:67])[CH:46]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 4

HCID 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 8177133-Bromo-5-methylpyridineHCID 86683895Tert-butyl cis-2-(6-amino-3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)pyridin-2-ylamino)cyclohexylcarbamate

Produkt 1

HCID 86683894
Tert-butyl cis-2-(3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)-6-(5-methylpyridin-3-ylamino)pyridin-2-ylamino)cyclohexylcarbamate
Ausbeute 55 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysatorHCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Xantphos (5 mg) and Pd2(dba)3 (4 mg) were added to a mixture of tert-butyl cis-2-(6-amino-3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)pyridin-2-ylamino)cyclohexylcarbamate (20 mg), cesium carbonate (20 mg), 3-bromo-5-methylpyridine (9 mg), and 1,4-dioxane (2 ml) in a nitrogen atmosphere, followed by reflux for 3 hours in a nitrogen atmosphere. The reaction mixture was cooled to room temperature, and water and ethyl acetate were added. The organic layer was collected, washed with saturated saline, and dried over anhydrous sodium sulfate, and the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel chromatography (silica gel: Kanto Chemical Co., Inc., silica gel 60 (spherical shape), hexane•ethyl acetate=2:1 to 3:1), and a white solid of tert-butyl cis-2-(3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)-6-(5-methylpyridin-3-ylamino)pyridin-2-ylamino)cyclohexylcarbamate (13 mg) was thus obtained.

Aufarbeitung

  1. temperatureby reflux for 3 hours in a nitrogen atmosphere
  2. customThe organic layer was collected
  3. washwashed with saturated saline
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled away under reduced pressure
  6. customThe obtained residue was purified by silica gel chromatography (silica gel: Kanto Chemical Co., Inc., silica gel 60 (spherical shape), hexane•ethyl acetate=2:1 to 3:1)

Quellen und Nachweise

ORD-Eintrag
ord-5f8f1123004047d89472b60cc8408d65
Quelldatensatz
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08772320B2

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