Benzene → 2-(N-alpha-chloroacetyl-2-methyl-3-methylthioanilino)acetaldehyde

HRID 1658971Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1658971
[CH3:1][C:2]1[C:11]([S:12][CH3:13])=[CH:10][CH:9]=[CH:8][C:3]=1[NH:4][CH2:5][CH:6]=[O:7].C(=O)([O-])[O-].[Na+].[Na+].C1C=CC=CC=1.[Cl:26][CH2:27][C:28](Cl)=[O:29]>O>[Cl:26][CH2:27][C:28]([N:4]([CH2:5][CH:6]=[O:7])[C:3]1[CH:8]=[CH:9][CH:10]=[C:11]([S:12][CH3:13])[C:2]=1[CH3:1])=[O:29]

Komponenten

6

Versuchsvorschrift

The dimethyl acetal of 2-(2-methyl-3-methylthioanilino)acetaldehyde (0.1 mole), sodium carbonate (0.06 mole) dissolved in water (50 ml) and benzene (50 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and cooling means. The mixture is cooled to a temperature of about 0°C and α-chloroacetyl chloride (0.11 mole) is incrementally added with stirring. After the addition is completed stirring is continued and the reaction mixture is permitted to warm to room temperature. After this time the mixture is filtered, washed with dilute hydrochloric acid and stripped of solvent to yield the desired product the dimethyl acetal of 2-(N-α-chloroacetyl-2-methyl-3-methylthioanilino)acetaldehyde.

Aufarbeitung

  1. customequipped with a mechanical stirrer
  2. temperaturethermometer and cooling means
  3. additionis incrementally added
  4. additionAfter the addition
  5. stirringis completed stirring
  6. filtrationAfter this time the mixture is filtered
  7. washwashed with dilute hydrochloric acid

Quellen und Nachweise

ORD-Eintrag
ord-9d81c8cac4d64ab48bc6edb5975ed8a1
Quelldatensatz
uspto-grants-1976_06
Patentnummer
US03966811

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