Hydroxide → Cymiazole

HRID 1679168Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1679168
[C:1]1([NH:9][C:10]([NH:12][CH3:13])=[S:11])[CH:6]=[CH:5][C:4]([CH3:7])=[CH:3][C:2]=1[CH3:8].C(OC(O[CH2:21][CH3:22])CCl)C.[OH-]>Cl>[C:1]1([N:9]=[C:10]2[N:12]([CH3:13])[CH:22]=[CH:21][S:11]2)[CH:6]=[CH:5][C:4]([CH3:7])=[CH:3][C:2]=1[CH3:8]

Komponenten

5

Edukt 3

HCID 961HydroxideHCID 121282-Chloro-1,1-diethoxyethaneHCID 30342141-(2,4-Dimethylphenyl)-3-methylthiourea

Produkt 1

HCID 43714Cymiazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

19.4 g (0.1 mole) of N-2,4-xylyl-N'-methyl-thiourea and 15.2 g (0.1 mole) of chloroacetaldehyde-diethylacetal in 150 ml of 2N aqueous hydrochloric acid are refluxed for 1 hour. The clear light-yellow solution is subsequently cooled to room temperature; it is rendered slightly alkaline with 30% aqueous medium hydroxide solution, and extracted with ether. The ether extract is washed with water, dried with sodium sulphate and filtered, and the ether is then distilled off. The oily residue is distilled; b.p. 132°-134° C/0.3 Torr; yield: 20.2 g = 92% of theory.

Aufarbeitung

  1. extractionextracted with ether
  2. extractionThe ether extract
  3. washis washed with water
  4. dry with materialdried with sodium sulphate
  5. filtrationfiltered
  6. distillationthe ether is then distilled off
  7. distillationThe oily residue is distilled

Quellen und Nachweise

ORD-Eintrag
ord-17326f4df40341ea967ed5534a26a618
Quelldatensatz
uspto-grants-1978_03
Patentnummer
US04079144

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