Sodium Bicarbonate → HCID 178512547, Verbindung

HRID 2292129Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2292129
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][CH2:9][S:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][CH:12]=1.[NH:18]([C:22]1[CH:30]=[CH:29][C:25]([C:26](Cl)=[O:27])=[CH:24][CH:23]=1)[C:19]([NH2:21])=[NH:20].[C:31]([O-:34])([OH:33])=[O:32].[Na+]>N1C=CC=CC=1>[C:31](=[O:32])([OH:34])[OH:33].[NH:18]([C:22]1[CH:30]=[CH:29][C:25]([C:26]([O:17][C:14]2[CH:13]=[CH:12][C:11]([S:10][CH2:9][CH2:8][O:7][CH:2]3[CH2:3][CH2:4][CH2:5][CH2:6][O:1]3)=[CH:16][CH:15]=2)=[O:27])=[CH:24][CH:23]=1)[C:19]([NH2:21])=[NH:20]

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 140519404-Hydroxyphenyl 2-(tetrahydropyran-2-yloxy)ethyl sulfide2×HCID 178512519HCID 178512519, Verbindung

Produkt 1

HCID 178512547HCID 178512547, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

96.08 g of 4-hydroxyphenyl 2-(tetrahydropyran-2-yloxy)ethyl sulfide synthesized by the above process (2) was dissolved in 800 ml of pyridine. 4-Guanidinobenzoyl chloride was added to the solution under cooling with ice and the mixture was stirred at room temperature for 24 h or longer. A saturated aqueous sodium hydrocarbonate solution was added thereto under cooling with ice and the precipitate thus obtained was recovered by filtration, washed with water, then acetone and finally ethyl acetate and dried to obtain 104 g of 4-(2-tetrahydropyran-2-yloxyethylthio)phenyl 4-guanidinobenzoate carbonate.

Aufarbeitung

  1. temperatureunder cooling with ice
  2. temperatureunder cooling with ice
  3. customthe precipitate thus obtained
  4. filtrationwas recovered by filtration
  5. washwashed with water
  6. dry with materialacetone and finally ethyl acetate and dried

Quellen und Nachweise

ORD-Eintrag
ord-420ad075b4ae453d9cdaca7d04116add
Quelldatensatz
uspto-grants-1989_01
Patentnummer
US04801603

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