Water → HCID 89835589, Verbindung

HRID 2277091Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2277091
[C:1]([O:4][C@H:5]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:6](Cl)=[O:7])(=[O:3])[CH3:2].C(N(CC)CC)C.[CH3:20][O:21][C:22]([C@@H:24]1[CH2:29][N:28]([CH3:30])[CH2:27][CH2:26][NH:25]1)=[O:23].O>C(Cl)Cl>[CH3:20][O:21][C:22]([C@@H:24]1[CH2:29][N:28]([CH3:30])[CH2:27][CH2:26][N:25]1[C:6](=[O:7])[C@H:5]([O:4][C:1](=[O:3])[CH3:2])[C:9]([CH3:12])([CH3:11])[CH3:10])=[O:23]

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 44141012(S)-methyl-4-methylpiperazine-2-carboxylateHCID 89824898HCID 89824898, Verbindung

Produkt 1

HCID 89835589HCID 89835589, VerbindungAusbeute 40,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a stirred solution of (2R)-1-chloro-3,3-dimethyl-1-oxobutan-2-yl acetate (0.247 g, 1.41 mmol) in CH2Cl2 (10 mL) was added triethylamine (0.39 mL, 2.83 mmol) and a solution of (S)-methyl-4-methylpiperazine-2-carboxylate (0.150 g, 0.943 mmol) in CH2Cl2 (3 mL) dropwise. The reaction mixture was stirred at room temperature for 30 minutes. Water (10 mL) was then added to quench the reaction and the reaction mixture was extracted with CH2Cl2 (2×25 mL). The combined organic layers were separated, washed with water (2×50 mL) dried over Na2SO4 and concentrated under reduced pressure to afford the title compound (0.12 g) as a white solid.

Aufarbeitung

  1. customto quench
  2. customthe reaction
  3. extractionthe reaction mixture was extracted with CH2Cl2 (2×25 mL)
  4. customThe combined organic layers were separated
  5. washwashed with water (2×50 mL)
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-f052adda9a9d43afa71a9b611c74f162
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09133147B2

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