Triethanolamine → N-(9-oxo-9H-thioxanthene-2-yl)methyl-N,N,N-tris(2-hydroxyethyl)ammonium bromide

HRID 533495

Reaktionsgleichung

[Br:1][CH2:2][C:3]1[CH:16]=[CH:15][C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6](=[O:17])[C:5]=2[CH:4]=1.[N:18]([CH2:25][CH2:26][OH:27])([CH2:22][CH2:23][OH:24])[CH2:19][CH2:20][OH:21]>ClCCl>[Br-:1].[O:17]=[C:6]1[C:5]2[CH:4]=[C:3]([CH2:2][N+:18]([CH2:25][CH2:26][OH:27])([CH2:22][CH2:23][OH:24])[CH2:19][CH2:20][OH:21])[CH:16]=[CH:15][C:14]=2[S:13][C:12]2[C:7]1=[CH:8][CH:9]=[CH:10][CH:11]=2

Komponenten

Reaktionsbedingungen

Temperatur: 25 °C

Versuchsvorschrift

The intermediate (C122-2-2) (2-bromomethylthioxanthone) (1.0 part) was dissolved in dichloromethane (85 g), and triethanol amine [product of Wako Pure Chemical industries, Ltd.] (0.5 parts) was added dropwise to this solution (an exotherm was observed after the addition). The resulting mixture was stirred at room temperature (about 25° C.) for one hour, and the organic solvent was evaporated under reduced pressure. As a result, 2.2 g of white solids were obtained. The white solids were recrystallized in a tetrahydrofuran/dichloromethane mixed solution, and 1.0 part of an intermediate (C122-2-3) was obtained (as brown solids).

Aufarbeitung

additionafter the addition)
customthe organic solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag: ord-1245c93b046441188adfc0390fd784f8
Quelldatensatz: uspto-grants-2014_10
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08853290B2

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