Methanesulfonyl chloride → N-{[4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}-N'-[1-(methylsulfonyl)piperidin-4-yl]urea

HRID 1371452Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1371452
[CH3:1][S:2](Cl)(=[O:4])=[O:3].Cl.[Cl:7][C:8]1[CH:9]=[C:10]([CH:29]=[CH:30][C:31]=1[Cl:32])[CH2:11][N:12]1[CH2:17][CH2:16][O:15][CH:14]([CH2:18][NH:19][C:20]([NH:22][CH:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)=[O:21])[CH2:13]1.C(N(CC)C(C)C)(C)C>ClCCl>[Cl:7][C:8]1[CH:9]=[C:10]([CH:29]=[CH:30][C:31]=1[Cl:32])[CH2:11][N:12]1[CH2:17][CH2:16][O:15][CH:14]([CH2:18][NH:19][C:20]([NH:22][CH:23]2[CH2:24][CH2:25][N:26]([S:2]([CH3:1])(=[O:4])=[O:3])[CH2:27][CH2:28]2)=[O:21])[CH2:13]1

Komponenten

5

Edukt 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 17984664HCID 17984664, Verbindung

Produkt 1

HCID 17984682N-{[4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}-N'-[1-(methylsulfonyl)piperidin-4-yl]urea

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
23 °C

Versuchsvorschrift

Methane sulphonyl chloride (0.009 ml) was added to a solution of Intermediate 16 (0.04 g) and N,N-diisopropylethylamine (0.048 ml) in dichloromethane (3 ml). The solution was stirred for 5 h at 23° C. The solvent was removed in vacuo and the residue was purified by solid phase extraction (Isolute SCX sulphonic acid column) eluting with methanol followed by 10% 0.880 ammonia solution in methanol, to give the title compound as a pale yellow gum (0.034 g).

Aufarbeitung

  1. customThe solvent was removed in vacuo
  2. customthe residue was purified by solid phase extraction (Isolute SCX sulphonic acid column)
  3. washeluting with methanol

Quellen und Nachweise

ORD-Eintrag
ord-de297dd2f4ad40578ef653e040a0dac3
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07157457B2

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