Isopropyl iodide → HCID 13365557, Verbindung

HRID 637294

Reaktionsgleichung

Reaktionsgleichung von HRID 637294
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:21])=[C:11]([N:15]4[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]4)[C:12]=3[F:14])[C:7](=[O:22])[C:6]([C:23]([OH:25])=[O:24])=[CH:5]2)[CH2:3][CH2:2]1.[CH:26]([I:29])([CH3:28])[CH3:27].C(N(CC)CC)C>CN(C)C=O>[IH:29].[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:21])=[C:11]([N:15]4[CH2:16][CH2:17][N:18]([CH:26]([CH3:28])[CH3:27])[CH2:19][CH2:20]4)[C:12]=3[F:14])[C:7](=[O:22])[C:6]([C:23]([OH:25])=[O:24])=[CH:5]2)[CH2:2][CH2:3]1

Komponenten

5

Edukt 3

HCID 6362Isopropyl iodideHCID 8471TriethylamineHCID 1228488-Fluorociprofloxacin

Produkt 1

HCID 13365557HCID 13365557, VerbindungAusbeute 44,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 3.5 g (0.01 mol) of 1-cyclopropyl-6,8-difluoro- 7-(piperazin-1-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 3.4 g (0.02 mol) of isopropyl iodide and 2.1 (0.02 mol) of triethylamine in 50 ml of dimethylformamide is heated to 80° C. in the course of 6 hours. After the solvent has been evaporated off, the residue is stirred with 30 ml of water and is then filtered off under suction, washed with water and recrystallised from methanol. 2.3 g of 1-cyclopropyl-6,8-difluoro-7-(4-isopropylpiperazin-1-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid hydriodide having a decomposition temperature of 306°-308° C. are obtained.

Aufarbeitung

  1. customAfter the solvent has been evaporated off
  2. filtrationis then filtered off under suction
  3. washwashed with water
  4. customrecrystallised from methanol

Quellen und Nachweise

ORD-Eintrag
ord-fbee618d44bd46c1800ec70fddfb1999
Quelldatensatz
uspto-grants-1985_12
Patentnummer
US04556658

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