Acetyl chloride → HCID 66745169, Verbindung

HRID 591653Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 591653
[CH:1]([NH:4][CH:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1)([CH3:3])[CH3:2].CCN(CC)CC.[C:25](Cl)(=[O:27])[CH3:26]>C(Cl)Cl>[CH:1]([N:4]([CH:5]1[CH2:6][CH2:7][N:8]([C:11]([O:13][C:14]([CH3:15])([CH3:17])[CH3:16])=[O:12])[CH2:9][CH2:10]1)[C:25](=[O:27])[CH3:26])([CH3:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 20801236tert-Butyl 4-[(propan-2-yl)amino]piperidine-1-carboxylate

Produkt 1

HCID 66745169HCID 66745169, VerbindungAusbeute 59,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a 0° C. solution of tert-butyl 4-(isopropylamino)piperidine-1-carboxylate (1.2 g, 5.19 mmol) in CH2Cl2 (18 mL) was added Et3N (1.44 mL, 10.38 mmol) followed by acetyl chloride (0.55 mL, 7.78 mmol). The resulting solution was stirred for 2.5 hours, then concentrated in vacuo. The material was purified by flash chromatography on silica gel, eluting with 0% to 5% of EtOAc/CH2Cl2, to afford tert-butyl 4-(N-isopropylacetamido)piperidine-1-carboxylate (0.88 g, 59%).

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. customThe material was purified by flash chromatography on silica gel
  3. washeluting with 0% to 5% of EtOAc/CH2Cl2

Quellen und Nachweise

ORD-Eintrag
ord-060ac4bd04dc4d37ab025f0b7a3d2459
Quelldatensatz
uspto-grants-2016_01
Patentnummer
US09238640B2

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