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Thioanisole → methyl (4S)-2-{5-(2-methoxyethoxy)-7-[methyl(pyridin-2-ylsulfonyl)amino]-1H-indol-2-yl}-4,5-dihydro-1,3-thiazole-4-carboxylate

HRID 504826
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 504826
C1(P(=O)(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.FC(F)(F)S(OS(C(F)(F)F)(=O)=O)(=O)=O.[CH3:36][O:37][C:38](=[O:89])[C@@H:39]([CH2:68][S:69]C(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[NH:40][C:41]([C:43]1[NH:44][C:45]2[C:50]([CH:51]=1)=[CH:49][C:48]([O:52][CH2:53][CH2:54][O:55][CH3:56])=[CH:47][C:46]=2[N:57]([CH3:67])[S:58]([C:61]1[CH:66]=[CH:65][CH:64]=[CH:63][N:62]=1)(=[O:60])=[O:59])=O.C1(SC)C=CC=CC=1.C(=O)([O-])O.[Na+]>ClCCl>[CH3:56][O:55][CH2:54][CH2:53][O:52][C:48]1[CH:49]=[C:50]2[C:45](=[C:46]([N:57]([CH3:67])[S:58]([C:61]3[CH:66]=[CH:65][CH:64]=[CH:63][N:62]=3)(=[O:60])=[O:59])[CH:47]=1)[NH:44][C:43]([C:41]1[S:69][CH2:68][C@H:39]([C:38]([O:37][CH3:36])=[O:89])[N:40]=1)=[CH:51]2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 7520ThioanisoleHCID 13097Triphenylphosphine OxideHCID 67749Trifluoromethanesulfonic anhydrideHCID 516892Sodium BicarbonateHCID 59135628N-({5-(2-methoxyethoxy)-7-[methyl(pyridin-2-ylsulfonyl)amino]-1H-indol-2-yl}carbonyl)-S-trityl-D-cysteine methyl ester

Produkt 1

HCID 57476261
methyl (4S)-2-{5-(2-methoxyethoxy)-7-[methyl(pyridin-2-ylsulfonyl)amino]-1H-indol-2-yl}-4,5-dihydro-1,3-thiazole-4-carboxylate
Ausbeute 98,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel3×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of triphenylphosphine oxide (1.3 g) in dichloromethane (3 mL) was added dropwise trifluoromethanesulfonic anhydride (0.59 mL) at 0° C., and the mixture was stirred at 0° C. for 15 min. The obtained suspension was diluted with dichloromethane (5 mL), and a solution of N-({5-(2-methoxyethoxy)-7-[methyl(pyridin-2-ylsulfonyl)amino]-1H-indol-2-yl}carbonyl)-S-trityl-D-cysteine methyl ester (0.60 g) and thioanisole (0.74 mL) in dichloromethane (8 mL) was added. The reaction mixture was stirred at 0° C. for 2 hr, and saturated aqueous sodium hydrogencarbonate solution was added. The mixture was concentrated, and the residue was extracted with ethyl acetate. The ethyl acetate layer was washed with water and saturated brine, dried (MgSO4), and concentrated. The obtained residue was subjected to silica gel column chromatography, and eluted with hexane-ethyl acetate (4:1-1:1, volume ratio) to give a mixture (0.39 g) of methyl (4S)-2-{5-(2-methoxyethoxy)-7-[methyl(pyridin-2-ylsulfonyl)amino]-1H-indol-2-yl}-4,5-dihydro-1,3-thiazole-4-carboxylate and triphenylphosphine oxide. The obtained mixture of the ester and triphenylphosphine oxide was dissolved in tetrahydrofuran (3 mL), sodium borohydride (0.010 mg) was added at 0° C., and methanol (1.5 mL) was added dropwise at 0° C. The reaction mixture was stirred at 0° C. for 30 min, and then at room temperature for 2 hr. Water was added, the mixture was concentrated, and the residue was extracted with ethyl acetate. The ethyl acetate layer was washed with water and saturated brine, dried (MgSO4), and concentrated. The obtained residue was subjected to basic silica gel column chromatography, and eluted with hexane-ethyl acetate-methanol (4:1:0-0:10:1, volume ratio) to give the title compound (0.076 g, yield 20%) as colorless crystals. melting point 146.6-146.7° C.

Aufarbeitung

  1. stirringThe reaction mixture was stirred at 0° C. for 2 hr
  2. concentrationThe mixture was concentrated
  3. extractionthe residue was extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with water and saturated brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. washeluted with hexane-ethyl acetate (4:1-1:1, volume ratio)

Quellen und Nachweise

ORD-Eintrag
ord-7a2d487294d44dfd9ebbc5373873539c
Quelldatensatz
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07777047B2

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