Triethylamine → HCID 22482356, Verbindung

HRID 2181904

Reaktionsgleichung

Reaktionsgleichung von HRID 2181904
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([S:9](Cl)(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1.[F:13][C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[CH:27]([NH2:29])[CH3:28].C(N(CC)CC)C>>[F:13][C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[CH:27]([NH:29][S:9]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=1)(=[O:11])=[O:10])[CH3:28]

Komponenten

4

Edukt 3

HCID 8471TriethylamineHCID 27375043-Methoxybenzenesulfonyl chlorideHCID 224822831-(2',5'-Difluoro-1,1'-biphenyl-2-yl)ethylamine

Produkt 1

HCID 22482356HCID 22482356, VerbindungAusbeute 94,2 %

Versuchsvorschrift

The title compound was prepared from 3-methoxybenzenesulfonyl chloride (326 mg, 1.6 mmol), 1-(-2′,5′-difluoro-biphenyl-2-yl)ethylamine (350 mg, 1.5 mmol), and triethylamine (418 μL, 3 mmol) according to the procedure and in the same manner as described in Example 112, step c. The product was purified by preparative liquid chromatography on a Biotage® 40 Mi column of prepacked silica gel (90 g), eluting with a gradient of 30%-50% methyl tert-butyl ether in hexane (35 min), to afford the desired compound (570 mg, 94%) as a clear glass;

Aufarbeitung

  1. customThe product was purified by preparative liquid chromatography on a Biotage® 40 Mi column of prepacked silica gel (90 g)
  2. washeluting with a gradient of 30%-50% methyl tert-butyl ether in hexane (35 min)

Quellen und Nachweise

ORD-Eintrag
ord-e392b8ea625a4ebbba7f86b7540ccb07
Quelldatensatz
uspto-grants-2005_05
Patentnummer
US06894061B2

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