6,7-Dibromo-8-nitro-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic acid → 8-Amino-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic acid

HRID 1413174Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1413174
Br[C:2]1[C:11](Br)=[C:10]([N+:13]([O-])=O)[C:5]2[O:6][CH2:7][CH2:8][O:9][C:4]=2[C:3]=1[C:16]([OH:18])=[O:17].[H][H]>[Pd].O>[NH2:13][C:10]1[C:5]2[O:6][CH2:7][CH2:8][O:9][C:4]=2[C:3]([C:16]([OH:18])=[O:17])=[CH:2][CH:11]=1

Komponenten

5

Edukt 2

HCID 205447596,7-Dibromo-8-nitro-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic acidHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 211934708-Amino-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic acidAusbeute 83,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

400 ml of water, 98.5 g of 6,7-dibromo-8-nitro-1,4-benzodioxane-5-carboxylic acid, 100 ml of soda and 10 g of Pd/c were introduced into an autoclave and then hydrogen under a pressure of 40 kg/cm2 was introduced while heating to 50° C. The mixture was filtered and then treated with 95 ml of hydrochloric acid. The precipitate was dried off, washed and dried. 42 g of 8-amino-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 186° C.; yield 83.7%).

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. additiontreated with 95 ml of hydrochloric acid
  3. customThe precipitate was dried off
  4. washwashed
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-0ba5cb6d35434a88a80f64308358b015
Quelldatensatz
uspto-grants-1981_02
Patentnummer
US04248885

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