Hydrochloric Acid → N-[(4-Methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]-3-(methoxymethyl)thiophene-2-sulfonamide

HRID 2352462Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2352462
[CH3:1][O:2][CH2:3][C:4]1[CH:8]=[CH:7][S:6][C:5]=1[S:9]([NH2:12])(=[O:11])=[O:10].[CH3:13][O:14][C:15]1[CH:20]=[C:19]([CH3:21])[N:18]=[C:17]([NH:22][C:23](=O)[O:24]C2C=CC=CC=2)[N:16]=1.Cl>O1CCOCC1>[CH3:13][O:14][C:15]1[CH:20]=[C:19]([CH3:21])[N:18]=[C:17]([NH:22][C:23]([NH:12][S:9]([C:5]2[S:6][CH:7]=[CH:8][C:4]=2[CH2:3][O:2][CH3:1])(=[O:11])=[O:10])=[O:24])[N:16]=1

Komponenten

5

Versuchsvorschrift

To 0.41 g of 3-(methoxymethyl)thiophene-2-sulfonamide and 0.52 g of phenyl N-(4-methoxy-6-methylpyrimidin-2-yl)carbamate in 25 mL of 1,4-dioxane is added 0.3 mL of 1,8-diazabicyclo[5.4]undec-7-ene. After being stirred for two hours at ambient temperature and pressure, the reaction mixture is poured onto 25-50 g of ice and the resultant mixture is acidified to pH 3 by the addition of hydrochloric acid. The desired solid product can be isolated by filtration. Alternatively, it can be extracted into methylene chloride which is then dried over magnesium sulfate, filtered and evaporated to dryness to yield the desired product in sufficiently pure form for the purposes of this invention.

Aufarbeitung

  1. customThe desired solid product can be isolated by filtration
  2. extractionAlternatively, it can be extracted into methylene chloride which
  3. dry with materialis then dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-87632bef14d44b769345923110a38f89
Quelldatensatz
uspto-grants-1989_10
Patentnummer
US04877440

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