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Ethyl ketone → Ethyl 2-{(3S,4R)-4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-[(1-ethylpropyl)amino]piperidin-1-yl}-1,3-benzothiazole-7-carboxylate

HRID 43851
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 43851
[CH3:1][CH2:2][C:3](=O)[CH2:4][CH3:5].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[NH2:21][C@@H:22]1[C@H:27]([NH:28][C:29]([C:31]2[NH:32][C:33]([CH2:37][CH3:38])=[C:34]([Cl:36])[N:35]=2)=[O:30])[CH2:26][CH2:25][N:24]([C:39]2[S:40][C:41]3[C:47]([C:48]([O:50][CH2:51][CH3:52])=[O:49])=[CH:46][CH:45]=[CH:44][C:42]=3[N:43]=2)[CH2:23]1.C(=O)(O)[O-].[Na+]>CO.O1CCCC1>[Cl:36][C:34]1[N:35]=[C:31]([C:29]([NH:28][C@@H:27]2[CH2:26][CH2:25][N:24]([C:39]3[S:40][C:41]4[C:47]([C:48]([O:50][CH2:51][CH3:52])=[O:49])=[CH:46][CH:45]=[CH:44][C:42]=4[N:43]=3)[CH2:23][C@@H:22]2[NH:21][CH:3]([CH2:4][CH3:5])[CH2:2][CH3:1])=[O:30])[NH:32][C:33]=1[CH2:37][CH3:38]
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Komponenten

7

Edukt 4

HCID 7288Ethyl ketoneHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 67548804Ethyl 2-[(3S,4R)-3-amino-4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}piperidin-1-yl]-1,3-benzothiazole-7-carboxylate

Produkt 1

HCID 67549801
Ethyl 2-{(3S,4R)-4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-[(1-ethylpropyl)amino]piperidin-1-yl}-1,3-benzothiazole-7-carboxylate
Ausbeute 68 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

3-Pentanone (68.9 μL, 0.65 mmol) and sodium triacetoxyborohydride (165 mg, 0.78 mmol) were added four times every two hours to a mixed solution of ethyl 2-[(3S,4R)-3-amino-4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}piperidin-1-yl]-1,3-benzothiazole-7-carboxylate obtained in Example (202e) (62.0 mg, 0.13 mmol) in methanol (1 mL) and tetrahydrofuran (1 mL) under ice-cooling, and the mixture was stirred at room temperature for 15 hours. Saturated aqueous sodium bicarbonate solution was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with brine and dried over anhydrous sodium sulfate. The insoluble matter was separated by filtration, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluate: hexane:ethyl acetate=1:1 v/v) to obtain 48 mg of the title compound (68%) as a colorless solid.

Aufarbeitung

  1. temperaturecooling
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe insoluble matter was separated by filtration
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe resulting residue was purified by silica gel column chromatography (eluate: hexane:ethyl acetate=1:1 v/v)

Quellen und Nachweise

ORD-Eintrag
ord-42193831b3294201acd2af812715ce45
Quelldatensatz
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08536197B2

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