Reaktion #94209

ord-00ff11ea7dbf4d609aa9e3c853244d07

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe precipitate is filtered off with suction
  2. 2
    Sonstigethe product is precipitated from the hot filtrate by the addition of water
  3. 3
    Filtrationsuction-filtered
  4. 4
    Waschenwashed with water
  5. 5
    Trocknenthe filtrate is dried with Na2SO4
  6. 6
    Einengenis then concentrated to dryness
  7. 7
    Sonstigeafter which process a further amount of the product is obtained
  8. 8
    Sonstigemelts at a temperature of from 198° to 200° C.
  9. 9
    Sonstigeis in the range of from 203° to 205° C.

Vorschrift

114 Grams (2.01 moles) of iron powder are added to a solution of 134 g (0.64 mole) of 5-chloro-6-nitro-1-indanone in 1600 ml of ethanol, then 63.5 ml of concentrated hydrochloric acid are added dropwise, and the reaction mixture is boiled for 4 hours. The precipitate is filtered off with suction, and the product is precipitated from the hot filtrate by the addition of water, then suction-filtered and washed with water. The residue of the reaction mixture is boiled with chloroform, the filtrate is dried with Na2SO4 and is then concentrated to dryness, after which process a further amount of the product is obtained. The substance melts at a temperature of from 198° to 200° C., and after recyrstallization from ethanol the melting point is in the range of from 203° to 205° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04129656uspto-grants-1978_12