Hydrochloric Acid → 7-Chloro-2,3-dihydro-1,4-benzodioxine-5-carboxylic acid

HRID 127420Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 127420
N[C:2]1[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=1.N([O-])=O.[Na+].[ClH:19]>O>[Cl:19][C:2]1[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric Acid2×HCID 205447527-Amino-2,3-dihydro-1,4-benzodioxine-5-carboxylic acidHCID 23668193Sodium Nitrite

Produkt 1

HCID 186136627-Chloro-2,3-dihydro-1,4-benzodioxine-5-carboxylic acidAusbeute 92,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

49 g of 7-amino-1,4-benzodioxane-5-carboxylic acid, 200 ml of water and 50 ml of hydrochloric acid were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was cooled to 5° C. and then a solution of 17.5 g of sodium nitrite in 38 ml of water was added. The suspension was then poured into a solution of 20 g of cuprous chloride in 75 ml of hydrochloric acid. The precipitate was dried off, washed and dissolved in a solution of 42 g of sodium bicarbonate in 420 ml of water. The solution was filtered and treated with 100 ml of hydrochloric acid. 50 g of 7-chloro-1,4-benzodioxane-5-carboxylic acid was produced (M.P.: 180° C.; yield: 92.7%).

Aufarbeitung

  1. customprovided with an agitator
  2. customThe precipitate was dried off
  3. washwashed
  4. dissolutiondissolved in a solution of 42 g of sodium bicarbonate in 420 ml of water
  5. filtrationThe solution was filtered
  6. additiontreated with 100 ml of hydrochloric acid

Quellen und Nachweise

ORD-Eintrag
ord-4f3bbf37f68643bc9484b828f58e88bb
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255580

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