2,2-Dimethoxy-1-methylpyrrolidine → 1-(4-Methoxyphenyl)-3-(1-methyl-2-pyrrolidinylidene)-2(1H,3H)-indolone

HRID 1110860

Reaktionsgleichung

Reaktionsgleichung von HRID 1110860
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][C:10]2=[O:18])=[CH:5][CH:4]=1.CO[C:21]1(OC)[CH2:25][CH2:24][CH2:23][N:22]1[CH3:26]>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=[C:21]3[CH2:25][CH2:24][CH2:23][N:22]3[CH3:26])[C:10]2=[O:18])=[CH:7][CH:8]=1

Komponenten

4

Edukt 2

HCID 110735522,2-Dimethoxy-1-methylpyrrolidineHCID 133395441-(4-Methoxyphenyl)-1,3-dihydro-2H-indol-2-one

Produkt 1

HCID 541264791-(4-Methoxyphenyl)-3-(1-methyl-2-pyrrolidinylidene)-2(1H,3H)-indolone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

1-(4-Methoxyphenyl)-2(1H,3H)-indolone (49 g, 0.205 mole), N-methyl-2-pyrrolidone dimethyl acetal (ca. 80%, 53 g, 0.245 mole, Ber, 97, pp. 3081-7, 1964) and 1000 ml chloroform were refluxed under nitrogen for 1.5 hours. The reaction mixture was cooled and evaporated in vacuo to solids. Two recrystallizations from ethyl acetate gave purified title product, 44.7 g, m.p. 90°-93° C. Thirty grams of this material were dried at 80° C/15 mm Hg for 20 hours to give 26.1 g of title product, m.p. 127°-9° C.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled
  2. customevaporated in vacuo to solids
  3. customTwo recrystallizations from ethyl acetate
  4. customgave
  5. custompurified title product, 44.7 g, m.p. 90°-93° C
  6. dry with materialThirty grams of this material were dried at 80° C/15 mm Hg for 20 hours

Quellen und Nachweise

ORD-Eintrag
ord-47b4ee654ed44417948272baf232cb0a
Quelldatensatz
uspto-grants-1990_12
Patentnummer
US04977178

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