Water → HCID 21412112, Verbindung

HRID 2071718

Reaktionsgleichung

Reaktionsgleichung von HRID 2071718
I[CH2:2][CH2:3][CH2:4][CH:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH:9]=[CH:8][C:7]2[CH:16]=[CH:17][CH:18]=[CH:19][C:6]1=2.CN(C)C=O.[C:25]1(=[O:35])[NH:29][C:28](=[O:30])[C:27]2=[CH:31][CH:32]=[CH:33][CH:34]=[C:26]12.[K].O>C(Cl)(Cl)Cl>[C:25]1(=[O:35])[N:29]([CH2:2][CH2:3][CH2:4][CH:5]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[CH:9]=[CH:8][C:7]3[CH:16]=[CH:17][CH:18]=[CH:19][C:6]2=3)[C:28](=[O:30])[C:27]2=[CH:31][CH:32]=[CH:33][CH:34]=[C:26]12

Komponenten

6

Versuchsvorschrift

5-(3-Iodopropyl)-5H-dibenzo[a,d]cycloheptene, 1.8 g. (0.005 mole), is dissolved in 10 ml. of dimethylformamide. The solution is stirred while 930 mg. (0.0051 mole) of potassium phthalimide is added. When the addition is complete, the mixture is heated to 85°-90° C. for 40 minutes, then cooled, diluted with chloroform and poured into water. The chloroform layer is separated and the aqueous layer extracted further with chloroform. Evaporation of the chloroform gives the product as an oily crystalline solid. Several recrystallizations from isopropyl alcohol gave product, m.p. 125.5°-131.5° C.

Aufarbeitung

  1. dissolution(0.005 mole), is dissolved in 10 ml
  2. additionWhen the addition
  3. temperaturethe mixture is heated to 85°-90° C. for 40 minutes
  4. temperaturecooled
  5. customThe chloroform layer is separated
  6. extractionthe aqueous layer extracted further with chloroform
  7. customEvaporation of the chloroform

Quellen und Nachweise

ORD-Eintrag
ord-3b5ba246c5794fba8c53474ff6c17a16
Quelldatensatz
uspto-grants-1977_09
Patentnummer
US04048223

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