Methylamine → HCID 15042211, Verbindung

HRID 974615Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 974615
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][CH:7]2[CH2:10][N:9]([C:11](Cl)=[O:12])[CH2:8]2)=[CH:4][CH:3]=1.[CH3:16][NH2:17]>O1CCCC1.O>[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][CH:7]2[CH2:10][N:9]([C:11]([NH:17][CH3:16])=[O:12])[CH2:8]2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 6329MethylamineHCID 15042229HCID 15042229, Verbindung

Produkt 1

HCID 15042211HCID 15042211, VerbindungAusbeute 85,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A stirred solution of 5 g (0.02 mole) of 3-(4-chlorophenoxy)-1-azetidinecarbonyl chloride in 20 ml of tetrahydrofuran was treated with 4.7 g (0.06 mole) of 40% aqueous monomethylamine. After stirring for 18 hr, the reaction mixture was diluted with 200 ml of water and the solid which separated was collected by filtration, 5.7 g. Recrystallization from benzene-ligroin was accomplished by adding magnesium sulfate to absorb the water which separated from the wet product. After filtering and cooling the hot filtrate, the precipitated solid was collected by filtration to yield 4.1 g (85.2%) of white crystals, m.p. 144°-145° C.

Aufarbeitung

  1. customthe solid which separated
  2. filtrationwas collected by filtration, 5.7 g
  3. customRecrystallization from benzene-ligroin
  4. additionby adding magnesium sulfate
  5. customto absorb the water which
  6. customseparated from the wet product
  7. filtrationAfter filtering
  8. temperaturecooling the hot filtrate
  9. filtrationthe precipitated solid was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-698fac724abe462b82098194420c7d0d
Quelldatensatz
uspto-grants-1991_11
Patentnummer
US05068231

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