Acryloyl chloride → HCID 178460006, Verbindung

HRID 370704

Reaktionsgleichung

Reaktionsgleichung von HRID 370704
Cl.Cl.[NH2:3][C:4]1[CH:12]=[CH:11][C:7]2[NH:8][N:9]=[N:10][C:6]=2[CH:5]=1.C(=O)([O-])O.[Na+].[C:18](Cl)([CH:20]=[CH2:21])=[O:19]>O>[C:18]([NH:3][C:4]1[CH:12]=[CH:11][C:7]2[NH:8][N:9]=[N:10][C:6]=2[CH:5]=1)(=[O:19])[CH:20]=[CH2:21]

Komponenten

5

Edukt 3

HCID 13140Acryloyl chlorideHCID 516892Sodium BicarbonateHCID 178478652HCID 178478652, Verbindung

Produkt 1

HCID 178460006HCID 178460006, VerbindungAusbeute 58,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

20.7 g of 5-aminobenzotriazole dihydrochloride and 30 g of sodium hydrogen carbonate were dissolved in 300 ml of water, and 10 g of acryl chloride was added dropwise at a temperature of lower than 10° C. over 20 minutes. After being stirred for 1 hour, the formed white precipitate was filtered off. Yield: 13.8 g. It was dissolved in 100 ml of DMF, and 500 ml of hot water at about 70° C. was added. It was immediately filtered under atmospheric pressure. The filtrate was allowed to cool, and the separated crystals were filtered out, washed with water and dried to obtain 11 g of the desired product which melted at 248°-253° C. The structure was confirmed by IR, NMR and elementary analysis.

Aufarbeitung

  1. filtrationthe formed white precipitate was filtered off
  2. dissolutionIt was dissolved in 100 ml of DMF
  3. addition500 ml of hot water at about 70° C. was added
  4. filtrationIt was immediately filtered under atmospheric pressure
  5. temperatureto cool
  6. filtrationthe separated crystals were filtered out
  7. washwashed with water
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-fd874fcb90364f05b78097c74f8e01c8
Quelldatensatz
uspto-grants-1985_07
Patentnummer
US04528264

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