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Toluene → 2(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(1 (R),2-dihydroxy-2-methyl-propyl)-pyrazin-2-yl]-propionamide

HRID 719978
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 719978
[C:1](=[O:4])([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:9]=[C:10]([C@@H:18]([CH2:32][CH:33]2[CH2:37][CH2:36][CH2:35][CH2:34]2)[C:19]([NH:21][C:22]2[CH:27]=[N:26][C:25](C=C(C)C)=[CH:24][N:23]=2)=[O:20])[CH:11]=[CH:12][C:13]=1[S:14]([CH3:17])(=[O:16])=[O:15].CS(N)(=O)=O.S([O-])([O-])=[O:44].[Na+].[Na+].[C:49]1([CH3:55])C=CC=C[CH:50]=1>C(OCC)(=O)C.[Fe-3](C#N)(C#N)(C#N)(C#N)(C#N)C#N.[K+].[K+].[K+].[Os](=O)(=O)(=O)=O.CC[C@@H]1[C@@H]2C[C@H]([C@@H](OC3C4C(=CC=CC=4)C(O[C@@H](C4C=CN=C5C=4C=C(OC)C=C5)[C@@H]4N5C[C@H](CC)[C@@H](CC5)C4)=NN=3)C3C=CN=C4C=3C=C(OC)C=C4)N(CC2)C1.O.C(O)(C)(C)C>[Cl:7][C:8]1[CH:9]=[C:10]([C@@H:18]([CH2:32][CH:33]2[CH2:34][CH2:35][CH2:36][CH2:37]2)[C:19]([NH:21][C:22]2[CH:27]=[N:26][C:25]([C@@H:1]([OH:4])[C:49]([OH:44])([CH3:55])[CH3:50])=[CH:24][N:23]=2)=[O:20])[CH:11]=[CH:12][C:13]=1[S:14]([CH3:17])(=[O:16])=[O:15]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 5

HCID 1140TolueneHCID 11430Potassium CarbonateHCID 24437Sodium SulfiteHCID 72879MethanesulfonamideHCID 674827762(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(2-methylpropenyl)-pyrazin-2-yl]-propionamide

Produkt 1

HCID 10480935
2(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(1 (R),2-dihydroxy-2-methyl-propyl)-pyrazin-2-yl]-propionamide
Ausbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 30318Osmium TetroxideKatalysatorHCID 112172021,4-Bis(dihydroquinidine)phthalazineKatalysatorHCID 178511488HCID 178511488, VerbindungKatalysatorHCID 8857Ethyl AcetateLösungsmittelHCID 714019492-Methylpropan-2-ol--water (1/1)Lösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

A mixture of potassium ferricyanide (738 mg, 2.24 mmol), potassium carbonate (310 mg, 2.24 mmol), and (DHQD)2PHAL (11.7 mg, 0.015 mmol) was treated with a solution of water/tert-butyl alcohol (15 mL, 1:1) and stirred at 25° C. to give a clear solution. The reaction mixture was then treated with a 0.2M solution of osmium tetroxide in toluene (37.4 μL). The reaction mixture was cooled to 0° C. and then was treated with 2(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(2-methylpropenyl)-pyrazin-2-yl]-propionamide (prepared as in Example 66, 345 mg, 0.748 mmol) followed by the addition of methane sulfonamide (71 mg, 0.747 mmol). The mixture was stirred at 0° C. for 18 h until all the olefin was reacted. The mixture was diluted with ethyl acetate (30 mL) and treated with sodium sulfite (1.0 g). The solution was extracted with ethyl acetate and water. The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 230–400 mesh, 1/5 hexanes/ethyl acetate) afforded 2(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(1(R),2-dihydroxy-2-methyl-propyl)-pyrazin-2-yl]-propionamide (328 mg, 89%) as an off-white foam: (ES)+-HRMS m/e calcd for C23H30ClN3O5S (M+H)+ 496.1668, found 496.1654.

Aufarbeitung

  1. customto give a clear solution
  2. temperatureThe reaction mixture was cooled to 0° C.
  3. customwas reacted
  4. extractionThe solution was extracted with ethyl acetate and water
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-be15350295a2472084898f1a077629ab
Quelldatensatz
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07132425B2

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