N-methyl-2-pyrrolidone → 2,2'-(Disulphanediyldiethane-2,1-diyl)bis(6-chloro-1H-benzo[de]-isoquinoline-1,3(2H)-dione)

HRID 2191174

Reaktionsgleichung

Reaktionsgleichung von HRID 2191174
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:16])O[C:8](=[O:15])[C:9]3[C:14]=2[C:13]=1[CH:12]=[CH:11][CH:10]=3.[ClH:17].[NH2:18][CH2:19][CH2:20][S:21][S:22][CH2:23][CH2:24][NH2:25].C(N([CH:32]([CH3:34])[CH3:33])CC)(C)C.CN1[CH2:40][CH2:39][CH2:38][C:37]1=[O:41]>>[S:21]([CH2:20][CH2:19][N:18]1[C:6](=[O:16])[C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[C:13]3[C:14]=2[C:9](=[CH:10][CH:11]=[CH:12]3)[C:8]1=[O:15])[S:22][CH2:23][CH2:24][N:25]1[C:8](=[O:15])[C:9]2[CH:34]=[CH:32][C:33]([Cl:17])=[C:11]3[C:10]=2[C:38](=[CH:39][CH:40]=[CH:12]3)[C:37]1=[O:41]

Komponenten

5

Edukt 4

HCID 13387N-methyl-2-pyrrolidone2×HCID 776721H,3H-Naphtho[1,8-cd]pyran-1,3-dione, 6-chloro-HCID 81531DiisopropylethylamineHCID 1676282-[(2-Aminoethyl)disulfanyl]ethan-1-amine hydrochloride

Produkt 1

HCID 594288842,2'-(Disulphanediyldiethane-2,1-diyl)bis(6-chloro-1H-benzo[de]-isoquinoline-1,3(2H)-dione)

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

9.30 g of 6-chloro-1H,3H-benzo[de]isochromene-1,3-dione and 4.46 g of hydrochlorided cystamine hydrochloride are suspended in 50 ml of N-methylpyrrolidone (NMP). 5.5 g of diisopropylethylamine are added and the mixture is heated with stirring at 120° C. After two hours, 50 ml of NMP are added and the mixture is kept with stirring at 120° C. for 3 hours. After cooling, the precipitated product is recovered and the filtered solution is extended by addition of 200 ml of water, and a second precipitate is recovered. The precipitates are washed with water and dried. 11.46 g of white powder are recovered. The analyses show that the product is in accordance with the expected product.

Aufarbeitung

  1. temperaturethe mixture is heated
  2. stirringwith stirring at 120° C. for 3 hours
  3. temperatureAfter cooling
  4. customthe precipitated product is recovered
  5. additionthe filtered solution is extended by addition of 200 ml of water
  6. customa second precipitate is recovered
  7. washThe precipitates are washed with water
  8. customdried
  9. custom11.46 g of white powder are recovered

Quellen und Nachweise

ORD-Eintrag
ord-bea679d39f5c448ebfbb5941ef2d50fe
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08328880B2

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