Potassium Hydroxide → 3-Methyl-6,7-bis(phenylmethoxy)quinoxaline-2-carboxylic acid
Reaktionsgleichung
[CH3:1][C:2]1[C:3]([C:28]([O:30]CC2C=CC=CC=2)=[O:29])=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][C:8]([O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[C:7]([O:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[CH:6]=2.[OH-].[K+]>C(O)C.O>[CH3:1][C:2]1[C:3]([C:28]([OH:30])=[O:29])=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][C:8]([O:12][CH2:13][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)=[C:7]([O:20][CH2:21][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)[CH:6]=2Komponenten
4
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
The compound of Example 27A (4.9 g, 10.0 mmol) was added to a solution of potassium hydroxide (2.2 g, 40.0 mmol) in ethanol/water (80 ml/16 ml) and the mixture was stirred at 80° C. for 20 hours and then cooled (5° C.). The precipitate was collected by suction, washed with ether (4.3 g) and then suspended in water (100 ml). After correction of the pH of this suspension to 2 by the addition of 2N HCl stirring was continued at room temperature for 20 minutes and the crystallized title compound was isolated by suction, washed with water and dried in vacuo over P2O5. Yield: 3.4 g (85%); mp 198°-200° C.
Aufarbeitung
- temperaturecooled (5° C.)
- customThe precipitate was collected by suction
- washwashed with ether (4.3 g)
- additionAfter correction of the pH of this suspension to 2 by the addition of 2N HCl stirring
- waitwas continued at room temperature for 20 minutes
- customthe crystallized title compound
- customwas isolated by suction
- washwashed with water
- dry with materialdried in vacuo over P2O5
Quellen und Nachweise
- ORD-Eintrag
- ord-bb5e63b0a78a4ab1baea0f2e61bd171d
- Quelldatensatz
- uspto-grants-1998_01
- Patentnummer
- US05705645
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