Sodium Hydroxide → 3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-ylmethyl)benzoic acid

HRID 1034071Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1034071
[OH-].[Na+].[CH:3]1[C:13]2[CH2:12][CH2:11][C:10]3[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=3[N:8]([CH2:18][C:19]3[CH:20]=[C:21]([CH:26]=[CH:27][CH:28]=3)[C:22]([O:24]C)=[O:23])[C:7]=2[CH:6]=[CH:5][CH:4]=1>O1CCOCC1.CO>[CH:14]1[C:10]2[CH2:11][CH2:12][C:13]3[CH:3]=[CH:4][CH:5]=[CH:6][C:7]=3[N:8]([CH2:18][C:19]3[CH:20]=[C:21]([CH:26]=[CH:27][CH:28]=3)[C:22]([OH:24])=[O:23])[C:9]=2[CH:17]=[CH:16][CH:15]=1

Komponenten

5

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

1N aqueous solution of sodium hydroxide (9 ml) was added to a solution of methyl 3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-ylmethyl)benzoate (1.06 g) in a mixture of 1,4-dioxane (25 ml) and methanol (15 ml) at 25° C. The mixture was stirred at 25° C. for 3 hours, and then at 50° C. for 30 minutes. After evaporation of the solvent, the residue was partitioned between ethyl acetate and 0.1N hydrochloric acid. The organic layer was separated, washed with water and brine, dried over magnesium sulfate, and evaporated to give 3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-ylmethyl)benzoic acid (1.01 g) as powder.

Aufarbeitung

  1. waitat 50° C. for 30 minutes
  2. customAfter evaporation of the solvent
  3. customthe residue was partitioned between ethyl acetate and 0.1N hydrochloric acid
  4. customThe organic layer was separated
  5. washwashed with water and brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-1eb71c34063a4e00b5abb32653d1c835
Quelldatensatz
uspto-grants-1994_05
Patentnummer
US05312829

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