Sodium Iodide → 4-Methoxycarbonylmethoxy-benzoic acid [1-methoxycarbonyl-2-(4-methoxy carbonyl methoxy-phenyl)-ethylcarbamoyl]-methoxycarbonylmethyl ester

HRID 2065439Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2065439
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH:9]([NH:14][C:15]([CH:17]([O:22][C:23](=[O:31])[C:24]2[CH:29]=[CH:28][C:27]([OH:30])=[CH:26][CH:25]=2)[C:18]([O:20][CH3:21])=[O:19])=[O:16])[C:10]([O:12][CH3:13])=[O:11])=[CH:4][CH:3]=1.[I-].[Na+].P(O)([O-])([O-])=O.[Na+].[Na+]>CC(C)=O>[CH3:13][O:12][C:10]([CH:9]([NH:14][C:15]([CH:17]([O:22][C:23](=[O:31])[C:24]1[CH:25]=[CH:26][C:27]([O:30][CH2:17][C:18]([O:20][CH3:21])=[O:19])=[CH:28][CH:29]=1)[C:18]([O:20][CH3:21])=[O:19])=[O:16])[CH2:8][C:5]1[CH:6]=[CH:7][C:2]([O:1][CH2:9][C:10]([O:12][CH3:13])=[O:11])=[CH:3][CH:4]=1)=[O:11]

Komponenten

5

Versuchsvorschrift

To a mixture of 4-hydroxy-benzoic acid [2-(4-hydroxy-phenyl)-1-methoxycarbonyl-ethyl carbamoyl]-methoxycarbonylmethyl ester 17 (10.7 grams, 24.82 mmol) anhydrous potassium carbonate (17.5 grams, 126.62 mmol), sodium iodide (3 grams, 20.01 mmol), and disodium phosphate (3 grams, 21.13 mmol) in anhydrous acetone (100 mL) is added methyl chloro acetate (7 grams, 64.5 mmol). The mixture is refluxed for 10 hours. Acetone is distilled off, and water (100 mL) is added. Crude 18 is filtered, dried, and can be purified in appropriate solvent.

Aufarbeitung

  1. temperatureThe mixture is refluxed for 10 hours
  2. distillationAcetone is distilled off
  3. additionwater (100 mL) is added
  4. filtrationCrude 18 is filtered
  5. customdried
  6. customcan be purified in appropriate solvent

Quellen und Nachweise

ORD-Eintrag
ord-478b562e8365463c85072657063fe3bd
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08288505B2

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