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Acetic Acid → HCID 59264610, Verbindung

HRID 646202
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 646202
[CH3:1][C:2]([N:9]1[CH2:14][CH2:13][C:12](=O)[CH2:11][CH2:10]1)([CH3:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[F:16][C:17]([F:33])([F:32])[C:18]1[CH:23]=[CH:22][C:21]([C:24]2[CH:29]=[CH:28][C:27]([CH2:30][NH2:31])=[CH:26][CH:25]=2)=[CH:20][CH:19]=1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>ClCCCl>[CH3:1][C:2]([N:9]1[CH2:14][CH2:13][CH:12]([NH:31][CH2:30][C:27]2[CH:26]=[CH:25][C:24]([C:21]3[CH:22]=[CH:23][C:18]([C:17]([F:16])([F:32])[F:33])=[CH:19][CH:20]=3)=[CH:29][CH:28]=2)[CH2:11][CH2:10]1)([CH3:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 176Acetic AcidHCID 10340Sodium CarbonateHCID 37291554-(4-Trifluoromethylphenyl)benzylamineHCID 5049666Sodium triacetoxyborohydrideHCID 59264612Ethyl 2-methyl-2-(4-oxo-1-piperidinyl)propanoate

Produkt 1

HCID 59264610HCID 59264610, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

A mixture of ethyl 2-methyl-2-(4-oxo-1-piperidinyl)propanoate (Int. A4) (25.6 g, 1.2 equiv), {[4′-(trifluoromethyl)-4-biphenylyl]methyl}amine (Int. A1) (31.1 g, 1.0 equiv), DCE (400 ml) and acetic acid (6.3 ml, 1.1 equiv) was stirred at room temperature under nitrogen. Sodium triacetoxyborohydride (33.5 g, 1.5 equiv) was added and stirring continued for 19 hours. Aqueous sodium carbonate (2M solution, excess) was added and stirred for 1.5 h, then the mixture was extracted with a mixture of diethyl ether and THF. The organic extracts were backwashed with water and brine, filtered through a pad of silica gel, dried over sodium sulfate and evaporated in vacuo. The desired product was obtained as a white solid (44.2 g) which was used without further purification.

Aufarbeitung

  1. stirringstirring
  2. stirringstirred for 1.5 h
  3. extractionthe mixture was extracted with a mixture of diethyl ether and THF
  4. filtrationfiltered through a pad of silica gel
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-ecc56f6bcdc4475b91163433d3844aa9
Quelldatensatz
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07705005B2

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