Methanol → 1,3-Bis(2-hydroxyethylthio)propane

HRID 258786

Reaktionsgleichung

Reaktionsgleichung von HRID 258786
[Na+].[SH-:2].[SH:3][CH2:4][CH2:5][OH:6].[CH3:7][O-:8].[Na+].Cl[CH2:11][CH2:12][CH2:13]Cl.[CH3:15]O>>[OH:6][CH2:5][CH2:4][S:3][CH2:11][CH2:12][CH2:13][S:2][CH2:15][CH2:7][OH:8]

Komponenten

6

Edukt 5

HCID 887MethanolHCID 15672-Mercaptoethanol2×HCID 88811,3-DichloropropaneHCID 28015Sodium hydrosulfideHCID 10942334Sodium Methoxide

Produkt 1

HCID 3737351,3-Bis(2-hydroxyethylthio)propaneAusbeute 95 %

Versuchsvorschrift

The sodium mercaptide of 2-mercaptoethanol was made by reacting 1 mole each of sodium methoxide and 2-mercaptoethanol in dry methanol under a nitrogen atmosphere. To this solution, 0.5 mole of 1,3-dichloropropane was added and the mixture was refluxed for 1 hour and filtered. The methanol filtrate was evaporated on a flash evaporator and traces of 2-mercaptoethanol were distilled off at high vacuum at room temperature. The yellow, oily residue was extracted with acetone, the solution filtered, and the acetone evaporated to give a 95 percent yield of the crude product.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 1 hour
  2. filtrationfiltered
  3. customThe methanol filtrate was evaporated on a flash evaporator and traces of 2-mercaptoethanol
  4. distillationwere distilled off at high vacuum at room temperature
  5. extractionThe yellow, oily residue was extracted with acetone
  6. filtrationthe solution filtered
  7. customthe acetone evaporated

Quellen und Nachweise

ORD-Eintrag
ord-b8a27b8a1a794ffebfedb31a6d6eee9a
Quelldatensatz
uspto-grants-1977_07
Patentnummer
USRE029305

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