Hydrochloric Acid → 8-Chloro-2,3-dihydro-1,4-benzodioxin-5-carboxylic acid
Reaktionsgleichung
N[C:2]1[C:7]2[O:8][CH2:9][CH2:10][O:11][C:6]=2[C:5]([C:12]([OH:14])=[O:13])=[CH:4][CH:3]=1.N([O-])=O.[Na+].[ClH:19]>O>[Cl:19][C:2]1[C:7]2[O:8][CH2:9][CH2:10][O:11][C:6]=2[C:5]([C:12]([OH:14])=[O:13])=[CH:4][CH:3]=1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 40 °C
Versuchsvorschrift
29.3 g of 8-amino-1,4-benzodioxane-5-carboxylic acid, 120 ml of water and 30 ml of hydrochloric acid were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was heated to 40° C. and then cooled to 5° C. and a solution of 10.5 g of sodium nitrite in 20 ml of water was added in portions with the temperature being maintained at from 5°-10° C. The mixture was agitated and then poured into a solution of 12 g of cuprous chloride in 45 ml of hydrochloric acid (d=1.18) with the temperature being maintained below 30° C. The precipitate was dried off, washed in 300 ml of water and 25 g of sodium bicarbonate. The solution was filtered and treated with hydrochloric acid. The precipitate was dried off, washed with water and dried. 20 g of 8-chloro-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 195° C.; yield: 62%).
Aufarbeitung
- customprovided with an agitator
- temperaturecooled to 5° C.
- temperaturebeing maintained at from 5°-10° C
- temperaturebeing maintained below 30° C
- customThe precipitate was dried off
- washwashed in 300 ml of water
- filtrationThe solution was filtered
- additiontreated with hydrochloric acid
- customThe precipitate was dried off
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-28429fa067de447d965b3f3ac7ff4edc
- Quelldatensatz
- uspto-grants-1981_03
- Patentnummer
- US04255580
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