Water → Methanesulfonic acid 1-pyrimidin-2-yl-piperidin-4-yl ester

HRID 1853372Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1853372
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][CH:10]([OH:13])[CH2:9][CH2:8]1.C(N(CC)CC)C.[CH3:21][S:22](Cl)(=[O:24])=[O:23].O>ClCCl>[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:8][CH2:9][CH:10]([O:13][S:22]([CH3:21])(=[O:24])=[O:23])[CH2:11][CH2:12]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 202340981-(Pyrimidin-2-yl)piperidin-4-ol

Produkt 1

HCID 86673125Methanesulfonic acid 1-pyrimidin-2-yl-piperidin-4-yl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a cooled solution of 1-Pyrimidin-2-yl-piperidin-4-ol (WO2008/8895 A1), (100 mg; 0.55 mmol) and triethylamine (233 μL, 1.67 mmol) in dry dichloromethane (1 mL), was added methanesulfonyl chloride (52 μL, 0.67 mmol). The reaction mixture was stirred at room temperature for 5 hours. Water was added. After extraction with dichloromethane, the combined organic extracts were dried over sodium sulfate and concentrated to afford a crude product that was used in the next step without further purification.

Aufarbeitung

  1. extractionAfter extraction with dichloromethane
  2. dry with materialthe combined organic extracts were dried over sodium sulfate
  3. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-eaf8a611c1f04dc9a9b81630d20d065e
Quelldatensatz
uspto-grants-2015_02
Patentnummer
US08962627B2

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