Reaktionsgleichung
[I:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH3:11])[CH:9]=[O:10])=[CH:4][CH:3]=1.S(=O)(=O)([OH:14])N.Cl([O-])=O.[Na+].S([O-])(O)=O.[Na+]>C(Cl)CCl.O>[I:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([CH3:11])[C:9]([OH:14])=[O:10])=[CH:6][CH:7]=1Komponenten
Versuchsvorschrift
To a solution of 34 g of 2-(4-iodophenyl)propionaldehyde in 100 ml of ethylene chloride was added a solution of 16.5 g of sulfamic acid in 85 ml of water. To the mixture was added dropwise with stirring a solution of 15.2 g of sodium chlorite in 22 ml of water, while maintaining the temperature at 10° to 15° C. After stirring for 10 minutes, about 15 g of sodium hydrogensulfite was added in small portions to the mixture. The organic layer was separated, washed with water, and mixed with 150 ml of 1 N sodium hydroxide solution. The aqueous layer was separated and adjusted to pH 3.0 with 6 N hydrochloric acid to precipitate white crystals. The crystals were collected by filtration, washed with water, and dried to obtain 34 g (94% yield) of 2-(4-iodophenyl)propionic acid.
Aufarbeitung
- additionTo the mixture was added dropwise
- temperaturewhile maintaining the temperature at 10° to 15° C
- customThe organic layer was separated
- washwashed with water
- additionmixed with 150 ml of 1 N sodium hydroxide solution
- customThe aqueous layer was separated
- customto precipitate white crystals
- filtrationThe crystals were collected by filtration
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-df16276f14824d189c533c6068590210
- Quelldatensatz
- uspto-grants-1980_10
- Patentnummer
- US04230719
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