Hydrochloric Acid → HCID 178490206, Verbindung

HRID 1817125Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1817125
[OH-:1].[Na+].[CH2:3]([SH:7])[C:4](O)=O.[CH3:8][O:9][C:10]1[CH:17]=[CH:16][C:13]([CH2:14]Cl)=[CH:12][C:11]=1[N+:18]([O-:20])=[O:19].Cl>CO>[CH3:8][O:9][C:10]1[CH:17]=[CH:16][C:13]([CH2:14][CH2:4][C:3]([OH:1])=[S:7])=[CH:12][C:11]=1[N+:18]([O-:20])=[O:19]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 1133Thioglycolic AcidHCID 14798Sodium HydroxideHCID 807854-(Chloromethyl)-2-nitroanisole

Produkt 1

HCID 178490206HCID 178490206, VerbindungAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a cold solution of sodium hydroxide (9.75 g, 240 mmol) in methanol (200 mL), thioglycollic acid (11.25 g, 120 mmol) was added slowly over 30 minutes. Sodium thioglycollate precipitated was dissolved by stirring and warming up the solution. The solution was cooled to room temperature and 4-methoxy-3-nitrobenzyl chloride (30.0 g, 120 mmol) was added in portions to reduce the intensity of exothermic reaction. The reaction mixture was then refluxed for 4 hours, cooled and poured onto crushed ice (1 Kg) containing hydrochloric acid (50 mL). The precipitate formed was filtered, washed with ice cold water and dried under vacuum. (30.0 g, 95% yield) m.p. 130-132° C.

Aufarbeitung

  1. customSodium thioglycollate precipitated
  2. dissolutionwas dissolved
  3. temperaturewarming up the solution
  4. customthe intensity of exothermic reaction
  5. temperatureThe reaction mixture was then refluxed for 4 hours
  6. temperaturecooled
  7. additionpoured
  8. customThe precipitate formed
  9. filtrationwas filtered
  10. washwashed with ice cold water
  11. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-6bddddafea5e4ed6be8462149801edd9
Quelldatensatz
uspto-grants-2009_10
Patentnummer
US07598232B2

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