1-Hydroxybenzotriazole → HCID 21959536, Verbindung

HRID 238462

Reaktionsgleichung

Reaktionsgleichung von HRID 238462
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:12]=1)[C:7]([OH:9])=O)([O-:3])=[O:2].[C:17]([N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1)([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18].C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C>C(Cl)Cl.C(Cl)CCl>[C:17]([N:24]1[CH2:25][CH2:26][N:27]([C:7]([C:6]2[CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)=[O:9])[CH2:28][CH2:29]1)([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18]

Komponenten

7

Edukt 4

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 6166023-Nitro-5-(trifluoromethyl)benzoic acid

Produkt 1

HCID 21959536HCID 21959536, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 111,2-DichloroethaneLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A mixture of 3-nitro-5-trifluoromethyl-benzoic acid (4.13 g), 4-Boc-piperazine (2.97 g), EDC (3.88 g), HOBt (2.74 g), DIEA (3.33 ml) in CH2Cl2 (120 ml) was stirred at RT for 3 h. The mixture was diluted with CH2Cl2 (100 ml), washed with sat'd NH4Cl, dried over MgSO4, filtered and concentrated. The residue was purified by silica gel chromatography (hexane, CH2Cl2:hexane 1:2) to give the compound as a white solid.

Aufarbeitung

  1. washwashed with sat'd NH4Cl
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel chromatography (hexane, CH2Cl2:hexane 1:2)

Quellen und Nachweise

ORD-Eintrag
ord-8cd5808f0eac4422a73836ee97f63108
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08642624B2

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