HCID 20284765, Verbindung → 4-Formyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole

HRID 127514

Reaktionsgleichung

Reaktionsgleichung von HRID 127514
[OH:1][CH2:2][C:3]#[C:4][CH2:5][S:6][C:7]1[NH:8][C:9]2[C:14]([CH:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2>N1C=CC=CC=1>[CH:2]([CH:3]1[C:15]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[NH:8][C:7]=2[S:6][CH2:5][CH2:4]1)=[O:1]

Komponenten

3

Edukt 1

HCID 20284765HCID 20284765, Verbindung

Produkt 1

HCID 147356294-Formyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indoleAusbeute 67,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

A solution of the product of the above (1) (12.0 g) in pyridine (120 ml) is heated at 100° C. for 2 hours and evaporated to remove the pyridine. The residue is dissolved in ether (300 ml), washed with water, 2 N hydrochloric acid and a saturated saline solution, dried and evaporated to remove the solvent. The residue (11.0 g) is chromatographed on silica gel (50 g) and eluted with benzene. The eluate is evaporated to give the title compound as an oil (8.14 g). The oil is gradually solidified in a refrigerator.

Aufarbeitung

  1. customevaporated
  2. customto remove the pyridine
  3. dissolutionThe residue is dissolved in ether (300 ml)
  4. washwashed with water, 2 N hydrochloric acid
  5. customa saturated saline solution, dried
  6. customevaporated
  7. customto remove the solvent
  8. customThe residue (11.0 g) is chromatographed on silica gel (50 g)
  9. washeluted with benzene
  10. customThe eluate is evaporated

Quellen und Nachweise

ORD-Eintrag
ord-92bc557fabfd4287adee9bad8db427cd
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04256640

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