Potassium Carbonate → HCID 86630319, Verbindung

HRID 19509

Reaktionsgleichung

Reaktionsgleichung von HRID 19509
[CH:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][N:2]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:17][S:18]([O:21][CH2:22][CH2:23][S:24][S:25][CH2:26][CH2:27]OS(C)(=O)=O)(=[O:20])=[O:19]>C(#N)C>[CH3:17][S:18]([O-:21])(=[O:20])=[O:19].[CH3:17][S:18]([O-:21])(=[O:20])=[O:19].[S:25]([CH2:26][CH2:27][N+:2]1[CH:3]=[CH:4][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[CH:1]=1)[S:24][CH2:23][CH2:22][N+:2]1[CH:3]=[CH:4][C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[CH:1]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 1190105,6,7,8-TetrahydroisoquinolineHCID 231172092-Methanesulfonyloxyethyl disulfide

Produkt 1

HCID 86630319HCID 86630319, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

3.2 g of 5,6,7,8-tetrahydroisoquinoline and 0.7 g of potassium carbonate were mixed in 3 ml of acetonitrile and brought to 80° C. A solution of 3.4 g of disulfanediyldiethane-2,1-diyl dimethane sulfonate in 3 ml of acetonitrile was added in 10 min. Stirring was maintained for 8 h at 80° C. and then the reaction medium was brought back to ambient temperature, filtered, and concentrated under vacuum. 6 ml of dichloromethane were added and the solution was poured dropwise into 500 ml of ethyl ether. The oil that had been separated by settling out was reprocessed twice by diluting in 6 ml of methanol and adding to 500 ml of ethyl ether, and a final time by diluting in 6 ml of dichloromethane and adding to 500 ml of ethyl ether. After drying under vacuum, 5.2 g of brown solid were recovered. The analyses were in compliance with the expected structure.

Aufarbeitung

  1. custombrought to 80° C
  2. customwas brought back to ambient temperature
  3. filtrationfiltered
  4. concentrationconcentrated under vacuum
  5. addition6 ml of dichloromethane were added
  6. additionthe solution was poured dropwise into 500 ml of ethyl ether
  7. customThe oil that had been separated
  8. additionby diluting in 6 ml of methanol
  9. additionadding to 500 ml of ethyl ether
  10. additiona final time by diluting in 6 ml of dichloromethane
  11. additionadding to 500 ml of ethyl ether
  12. dry with materialAfter drying under vacuum, 5.2 g of brown solid
  13. customwere recovered

Quellen und Nachweise

ORD-Eintrag
ord-cd1ca81fc66c4efbb1f88f5beb425df2
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07744657B2

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