Tetrahydrofuran → HCID 178482395, Verbindung

HRID 450334Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 450334
[CH3:1][NH:2][C:3]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:6]([C:7]([OH:9])=O)=[C:5]([N:15]2[CH2:20][CH2:19][CH:18]([C:21]([F:24])([F:23])[F:22])[CH2:17][CH2:16]2)[N:4]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C1COCC1.[F:52][C:53]([F:62])([F:61])[C@H:54]1[CH2:59][CH2:58][C@H:57]([NH2:60])[CH2:56][CH2:55]1>O.CN(C=O)C>[F:52][C:53]([F:61])([F:62])[C@H:54]1[CH2:55][CH2:56][C@H:57]([NH:60][C:7](=[O:9])[C:6]2[CH:10]=[C:11]([N+:12]([O-:14])=[O:13])[C:3]([NH:2][CH3:1])=[N:4][C:5]=2[N:15]2[CH2:20][CH2:19][CH:18]([C:21]([F:23])([F:24])[F:22])[CH2:17][CH2:16]2)[CH2:58][CH2:59]1

Komponenten

7

Edukt 4

HCID 8028TetrahydrofuranHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 679584096-Methylamino-5-nitro-2-(4-trifluoromethyl-piperidinyl)-nicotinic acidHCID 178511531HCID 178511531, Verbindung

Produkt 1

HCID 178482395HCID 178482395, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 6-methylamino-5-nitro-2-(4-trifluoromethyl-piperidinyl)-nicotinic acid (570 mg, 1.64 mmol), TBTU (540 mg, 1.68 mmol), TEA (1.00 mL, 7.2 mmol), THF (10 mL) and DMF (5 mL) are stirred for 5 min. Then trans-4-trifluoromethyl-cyclohexylamine (335 mg, 1.65 mmol) is added and it is stirred for 30 min. Water is added, the mixture is concentrated and the precipitate is filtered, washed with water and dried at 55° C.

Aufarbeitung

  1. stirringit is stirred for 30 min
  2. concentrationthe mixture is concentrated
  3. filtrationthe precipitate is filtered
  4. washwashed with water
  5. customdried at 55° C.

Quellen und Nachweise

ORD-Eintrag
ord-ef2e87da43b24340965ab2eb288af87d
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08486968B2

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