Potassium Carbonate → HCID 178418231, Verbindung

HRID 1458256

Reaktionsgleichung

Reaktionsgleichung von HRID 1458256
[CH3:1][O:2][N:3]=[C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([C:15]([OH:17])=O)[C:12]=2[CH3:14])[S:7](=[O:19])(=[O:18])[CH2:6][CH2:5]1.[CH2:20]([N:22]1[C:26]([OH:27])=[CH:25][CH:24]=[N:23]1)[CH3:21].C(=O)([O-])[O-].[K+].[K+]>C(O)(CC)(C)C>[CH3:1][O:2][N:3]=[C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([C:15]([C:25]3[CH:24]=[N:23][N:22]([CH2:20][CH3:21])[C:26]=3[OH:27])=[O:17])[C:12]=2[CH3:14])[S:7](=[O:19])(=[O:18])[CH2:6][CH2:5]1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 539715404-Methoxyimino-5-methylthiochroman-6-carboxylic acid-1,1-dioxideHCID 178418331HCID 178418331, Verbindung

Produkt 1

HCID 178418231HCID 178418231, VerbindungAusbeute 72,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 64052-Methyl-2-butanolLösungsmittel

Versuchsvorschrift

0.9 Gram (3.2 mmol) of the 4-methoxyimino-5-methylthiochroman-6-carboxylic acid-1,1-dioxide and 0.44 g (3.9 mmol) of 1-ethyl-5-hydroxypyrazol were dissolved in 5 ml of t-amyl alcohol, and 0.81 g (3.9 mmol) of DCC(dicyclohexyl-carbodiimide) was added at room temperature. The mixture was stirred at room temperature for 2 hours, then, 0.74 g (5.4 mmol) of potassium carbonate was added, and the mixture was allowed to react at 90° C. for 8 hours. After the reaction, the solvent was distilled off, ethyl acetate was added, and the mixture was extracted with a 5% potassium carbonate aqueous solution. An aqueous layer was neutralized with concentrated hydrochloric acid, and extracted with ethyl acetate. The extract was washed with a saturated sodium hydroxide aqueous solution, dried over sodium sulfate and concentrated to give 0.88 g (yield 72%) of 4-methoxyimino-5-methyl-6 -(1-ethyl-5-hydroxypyrazol-4-yl)carbonylthiochroman-1,1-dioxide.

Aufarbeitung

  1. customto react at 90° C. for 8 hours
  2. customAfter the reaction
  3. distillationthe solvent was distilled off
  4. additionethyl acetate was added
  5. extractionthe mixture was extracted with a 5% potassium carbonate aqueous solution
  6. extractionextracted with ethyl acetate
  7. washThe extract was washed with a saturated sodium hydroxide aqueous solution
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-de65b6be9942400f8d6080f2f3e6e3b6
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05849926

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