Benzene → HCID 53654230, Verbindung

HRID 1973956Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1973956
Cl.[NH:2]=[C:3]1[CH2:7][CH2:6][CH2:5][N:4]1[CH3:8].C1C=CC=CC=1.[OH-].[Na+].[C:17]1([CH3:26])[C:18]([N:23]=[C:24]=[O:25])=[CH:19][CH:20]=[CH:21][CH:22]=1>O>[CH3:8][N:4]1[CH2:5][CH2:6][CH2:7][C:3]1=[N:2][C:24]([NH:23][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[CH3:26])=[O:25]

Komponenten

6

Edukt 4

HCID 241BenzeneHCID 14798Sodium HydroxideHCID 691942-Tolyl isocyanateHCID 124489671-Methylpyrrolidin-2-imine hydrochloride

Produkt 1

HCID 53654230HCID 53654230, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A 6.73 g. (0.05 mole) sample of 2-imino-1-methylpyrrolidine HCl is treated with 50 ml. of benzene and 2 ml. of water. With stirring, 10 ml. of 50% sodium hydroxide is added. After stirring about one minute, the benzene layer is decanted onto anhydrous K 2 CO 3 and the extraction repeated twice with 50 ml. portions of benzene. The dried, combined extracts are filtered from the drying agent and the filtrate is treated with 6.66 g. (0.05 mole) of o-tolylisocyanate. After stirring overnight, the mixture is filtered from a small amount of insoluble material and the solvent removed in vacuo. Recrystallization from ethyl acetate and finally from ether gives the pure product, 1-(1-methyl-2-pyrrolidylidene)-3-o-tolyl urea, m.p. = 91°- 93° C.

Aufarbeitung

  1. stirringAfter stirring about one minute
  2. customthe benzene layer is decanted onto anhydrous K 2 CO 3
  3. extractionthe extraction
  4. filtrationare filtered from the drying agent
  5. additionthe filtrate is treated with 6.66 g
  6. stirringAfter stirring overnight
  7. filtrationthe mixture is filtered from a small amount of insoluble material
  8. customthe solvent removed in vacuo
  9. customRecrystallization from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-10e93bd9fe2143cfaa270185382eefc1
Quelldatensatz
uspto-grants-1976_12
Patentnummer
US03998958

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