Triethylamine → 2-[2-(4-Methylpiperazino)-2-oxoethyl]phenyl N-octadecylcarbamate

HRID 1250779Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1250779
C(N(CC)CC)C.[CH2:8]([N:26]=[C:27]=[O:28])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].[OH:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[CH2:36][C:37]([N:39]1[CH2:44][CH2:43][N:42]([CH3:45])[CH2:41][CH2:40]1)=[O:38]>C(Cl)Cl>[CH2:8]([NH:26][C:27](=[O:28])[O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[CH2:36][C:37]([N:39]1[CH2:44][CH2:43][N:42]([CH3:45])[CH2:41][CH2:40]1)=[O:38])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 66988Octadecyl isocyanateHCID 18520258HCID 18520258, Verbindung

Produkt 1

HCID 185202532-[2-(4-Methylpiperazino)-2-oxoethyl]phenyl N-octadecylcarbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Triethylamine (1.06 ml) and octadecyl isocyanate (2.35 ml) were added to a solution containing 2-(2-hydroxyphenyl)-1-(4-methylpiperazino)-1-ethanone (1.60 g) in methylene chloride (16 ml) and stirred for 15.5 hours at room temperature. The insoluble matters were filtrated out and washed with chloroform. The filtrate and washings were combined and the mixture was washed with saturated sodium hydrogencarbonate aqueous solution and brine successively, dried over sodium sulfate anhydride, and concentrated. The residue was purified by silica gel column chromatography (silica gel 100 g, chloroform:methanol=50:1 to 30:1), thereby yielding the entitled compound (3.23 g) as white solid.

Aufarbeitung

  1. filtrationThe insoluble matters were filtrated out
  2. washwashed with chloroform
  3. washthe mixture was washed with saturated sodium hydrogencarbonate aqueous solution and brine successively
  4. dry with materialdried over sodium sulfate anhydride
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (silica gel 100 g, chloroform:methanol=50:1 to 30:1)

Quellen und Nachweise

ORD-Eintrag
ord-a2ec2b0c41fe480ca06d4047fc235ee7
Quelldatensatz
uspto-grants-2002_01
Patentnummer
US06339154B1

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