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Diisopropylethylamine → (2E)-2-(3-chloro-4-methylsulfonylphenyl)-2-cyclopentyloxyimino-N-(3-methyl-1,2,4-thiadiazol-5-yl)acetamide

HRID 600966
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 600966
[Cl:1][C:2]1[CH:3]=[C:4](/[C:12](=[N:22]\[O:23][CH:24]2[CH2:28][CH2:27][CH2:26][CH2:25]2)/[C:13]([NH:15][C:16]2C=CN(C)[N:17]=2)=[O:14])[CH:5]=[CH:6][C:7]=1[S:8]([CH3:11])(=[O:10])=[O:9].[CH3:29][C:30]1N=C(N)[S:32][N:31]=1.C(N(CC)C(C)C)(C)C>C(#N)C>[Cl:1][C:2]1[CH:3]=[C:4](/[C:12](=[N:22]\[O:23][CH:24]2[CH2:25][CH2:26][CH2:27][CH2:28]2)/[C:13]([NH:15][C:16]2[S:32][N:31]=[C:30]([CH3:29])[N:17]=2)=[O:14])[CH:5]=[CH:6][C:7]=1[S:8]([CH3:11])(=[O:10])=[O:9]
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Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 3506395-Amino-3-methyl-1,2,4-thiadiazoleHCID 59745110(2E)-2-(3-chloro-4-methylsulfonylphenyl)-2-cyclopentyloxyimino-N-(1-methylpyrazol-3-yl)acetamide

Produkt 1

HCID 87416799(2E)-2-(3-chloro-4-methylsulfonylphenyl)-2-cyclopentyloxyimino-N-(3-methyl-1,2,4-thiadiazol-5-yl)acetamideAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342
Acetonitrile
Lösungsmittel

Versuchsvorschrift

(E)-(3-Chloro-4-methanesulfonyl-phenyl)-cyclopentyloxyimino-acetic (prepared as in Example 1, 96 mg, 0.28 mmol), 3-methyl-[1,2,4]thiadiazol-5-ylamine (32 mg, 0.28 mmol) and N,N-diisopropylethylamine (145 μL, 0.83 mmol) were combined in acetonitrile (1.25 mL) and cooled in an ice bath. O-(7-Azabenzotriazole-1-yl)-N,N,N′N′-tetramethyluronium hexafluorophosphate (106 mg, 0.28 mmol) was added and the ice bath was removed. After stirring 2 h, the reaction mixture was evaporated in vacuo. The residue was treated with saturated aqueous sodium bicarbonate solution (1 mL) and extracted with chloroform (2×3 mL). The combined organic phases were dried over sodium sulfate and evaporated in vacuo. The residue was purified by flash column chromatography (Merck silica gel 60, 40-63 μm; 40% ethyl acetate/hexanes) to afford (E)-2-(3-chloro-4-methanesulfonyl-phenyl)-2-cyclopentyloxyimino-N-(3-methyl-[1,2,4]thiadiazol-5-yl)-acetamide (62 mg, 50%) as a white solid after lyophilization from aqueous acetonitrile: LC-MS (ESI) m/e calcd for C17H19ClN4O4S2 [M+] 442.05, found 443 [M+H+]; H1-NMR (400 MHz, CDCl3) δ ppm 1.67 (m, 4 H, 2×CH2), 1.90 (m, 4 H, 2×CH2), 2.60 (s, 3 H, ArCH3), 3.32 (s, 3 H, SO2CH3), 4.95 (m, 1 H, OCH), 7.60 (dd, Jo=8.3, Jm=1.6 Hz, 1 H, Ar), 7.70 (d, Jm=1.6 Hz, 1 H, Ar), 8.22 (d, Jo=8.3 Hz, 1 H, Ar), 10.35 (s, 1 H, NH).

Aufarbeitung

  1. temperaturecooled in an ice bath
  2. customthe ice bath was removed
  3. customthe reaction mixture was evaporated in vacuo
  4. additionThe residue was treated with saturated aqueous sodium bicarbonate solution (1 mL)
  5. extractionextracted with chloroform (2×3 mL)
  6. dry with materialThe combined organic phases were dried over sodium sulfate
  7. customevaporated in vacuo
  8. customThe residue was purified by flash column chromatography (Merck silica gel 60, 40-63 μm; 40% ethyl acetate/hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-bffe805ea1fb4838bf6154dc42ffefb9
Quelldatensatz
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07902248B2

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