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Sodium Hydroxide → 5-(Dimethylamino)methyl-2-mercaptomethyl-4-methylthiophene

HRID 236254
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 236254
Cl.Cl.C([S:6][CH2:7][C:8]1[S:9][C:10]([CH2:14][N:15]([CH3:17])[CH3:16])=[C:11]([CH3:13])[CH:12]=1)(=N)N.[OH-].[Na+]>O>[CH3:17][N:15]([CH2:14][C:10]1[S:9][C:8]([CH2:7][SH:6])=[CH:12][C:11]=1[CH3:13])[CH3:16]
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Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 138252712-Amidinothiomethyl-5-(dimethylamino)methyl-4-methylthiophene dihydrochloride

Produkt 1

HCID 138252725-(Dimethylamino)methyl-2-mercaptomethyl-4-methylthiopheneAusbeute 83,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

In 5 ml of water was dissolved 10 g of 2-amidinothiomethyl-5-(dimethylamino)methyl-4-methylthiophene dihydrochloride, and 2.52 g of sodium hydroxide was added thereto, and the resulting mixture was subjected to reaction under reflux for 2.5 hours in a nitrogen atmosphere. The reaction mixture was cooled to room temperature, and then extracted with 100 ml of methylene chloride, and the extract was dried over anhydrous magnesium sulfate, after which the solvent was removed by distillation under reduced pressure. The oily substance thus obtained was distilled under reduced pressure in a nitrogen atmosphere to obtain 5.3 g (yield 83%) of 5-(dimethylamino)methyl-2-mercaptomethyl-4-methylthiophene having a boiling point of 102°-105° C./3 mmHg.

Aufarbeitung

  1. additionwas added
  2. customthe resulting mixture was subjected to reaction
  3. temperatureunder reflux for 2.5 hours in a nitrogen atmosphere
  4. extractionextracted with 100 ml of methylene chloride
  5. dry with materialthe extract was dried over anhydrous magnesium sulfate
  6. customafter which the solvent was removed by distillation under reduced pressure
  7. customThe oily substance thus obtained
  8. distillationwas distilled under reduced pressure in a nitrogen atmosphere

Quellen und Nachweise

ORD-Eintrag
ord-ec12ae60b06b41c0803eb80d956fb700
Quelldatensatz
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04643849

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