Water → HCID 131723643, Verbindung

HRID 1018588Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1018588
[F:1][C:2]([F:34])([F:33])[C:3]1[CH:4]=[C:5]([CH:26]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:28]=1)[C:6]([N:8]1[CH2:25][CH2:24][C:11]2([N:15]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH:14]([CH3:22])[NH:13][C:12]2=[O:23])[CH2:10][CH2:9]1)=[O:7].[H-].[Na+].[Cl-].ClC[C:40]1[CH:41]=[NH+:42][CH:43]=[CH:44][CH:45]=1.O.[CH3:47]N(C)C=O>>[F:34][C:2]([F:1])([F:33])[C:3]1[CH:4]=[C:5]([CH:26]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:28]=1)[C:6]([N:8]1[CH2:9][CH2:10][C:11]2([N:15]([C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:14]([CH3:47])([CH3:22])[N:13]([C:40]3[CH:41]=[N:42][CH:43]=[CH:44][CH:45]=3)[C:12]2=[O:23])[CH2:24][CH2:25]1)=[O:7]

Komponenten

6

Edukt 5

HCID 962WaterHCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 10184617HCID 10184617, VerbindungHCID 438334963-Picolyl chloride hydrochloride

Produkt 1

HCID 131723643HCID 131723643, VerbindungAusbeute 93 %

Versuchsvorschrift

(rac)-8-(3,5-Bis-trifluoromethyl-benzoyl)-2-methyl-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one (200 mg, 0.41 mmol) was dissolved in dimethyl formamide (10 mL) and sodium hydride (40 mg, 60% in mineral oil, 1 mmol) and 3-chloromethyl pyridinium chloride (82 mg, 0.5 mmol) were added and stirred at room temperature overnight. Water (30 mL) was added and the reaction mixture extacted with ethyl actetate. The organic phases were pooled, dried with MgSO4 and the solvent was evaporated. The residue was purified by chromatography on silica gel (ethyl acetate) to yield the desired product (219 mg, 93%), MS: m/e=577.0 (M+H+).

Aufarbeitung

  1. dry with materialdried with MgSO4
  2. customthe solvent was evaporated
  3. customThe residue was purified by chromatography on silica gel (ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-1923056442544e5893602bb2419e4a43
Quelldatensatz
uspto-grants-2002_11
Patentnummer
US06482829B2

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