Reaktion #346220

ord-06cbda73d51744e388e380869a3b6119

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeis collected on
  2. 2
    Filtrationa filter
  3. 3
    Waschenwashed with ether
  4. 4
    ExtraktionThe filtrate is extracted with 2% aqueous HCl
  5. 5
    Extraktionextracted with chloroform
  6. 6
    ExtraktionThe chloroform extract
  7. 7
    Trocknenis dried (MgSO4)
  8. 8
    Filtrationfiltered
  9. 9
    Sonstigeevaporated

Vorschrift

A solution of the amide of formula 3, N,N,4-trimethyl-4H-pyrrolo-[2,1-c][1,4]benzoxazine-4-carboxamide (3 g), described in Example 15 in 50 ml of ether is added dropwise to a suspension of lithium aluminum hydride (1.5 g) in anhydrous ether (100 ml) over a period of 30 min. The reaction mixture is stirred at room temperature for 16 hr. Decomposition of the mixture with 6 ml of water gives a white precipitate, which is collected on a filter and washed with ether. The filtrate is extracted with 2% aqueous HCl. The extract is rendered basic with a 10% solution of NaOH and extracted with chloroform. The chloroform extract is dried (MgSO4), filtered and evaporated to give the title compound, nmr (DMSO-d6) δ 1.85 (s, 3H), 2.78 (s, 6H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04035495uspto-grants-1977_07