Methylamine → 3-(3,4-Dichlorophenoxy)-N-methylazetidine-1-carboxamide

HRID 974607Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 974607
[Cl:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[Cl:16])[O:5][CH:6]1[CH2:9][N:8]([C:10](Cl)=[O:11])[CH2:7]1.[CH3:17][NH2:18]>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[Cl:16])[O:5][CH:6]1[CH2:9][N:8]([C:10]([NH:18][CH3:17])=[O:11])[CH2:7]1

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 15042235HCID 15042235, Verbindung

Produkt 1

HCID 150422213-(3,4-Dichlorophenoxy)-N-methylazetidine-1-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 5.6 g (0.02 mole) of 3-(3,4-dichlorophenoxy)-1-azetidinecarbonyl chloride in 20 ml of tetrahydrofuran was stirred while 5 ml (0.06 mole) of 40% aqueous methylamine was added slowly, stirring was continued for 18 hr. The reaction mixture was diluted with 200 ml of ice water, and the solid which formed was collected by filtration, 6.9 g. The crude wet solid was recrystallized from ethanol/water to yield 3.65 g (66.3%) of greenish-gray plate-like crystals, m.p. 158°-159° C.

Aufarbeitung

  1. additionwas added slowly
  2. customthe solid which formed
  3. filtrationwas collected by filtration, 6.9 g
  4. customThe crude wet solid was recrystallized from ethanol/water
  5. customto yield 3.65 g (66.3%) of greenish-gray plate-like crystals, m.p. 158°-159° C.

Quellen und Nachweise

ORD-Eintrag
ord-6f5707f449a545f9b0015457f8f61c6d
Quelldatensatz
uspto-grants-1991_11
Patentnummer
US05068231

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