Methanethiol → Methylmercapto-2-chlorocyclohexanone

HRID 2294766

Reaktionsgleichung

Reaktionsgleichung von HRID 2294766
[Cl:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C:3]1=[O:8].[Na].[CH3:10][SH:11].O>C(O)C>[CH3:10][S:11][C:2]1([Cl:1])[CH2:7][CH2:6][CH2:5][CH2:4][C:3]1=[O:8]

Komponenten

6

Edukt 4

HCID 878MethanethiolHCID 962WaterHCID 132032-ChlorocyclohexanoneHCID 5360545Sodium

Produkt 1

HCID 54407380Methylmercapto-2-chlorocyclohexanoneAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

In a 300-ml egg-plant type flask 7.07 g (0.053 mol) of 2-chlorocyclohexanone was dissolved in 50 ml of ethanol, and 25 ml of 15% aqueous solution of sodium salt of methylmercaptan was added dropwise with a dropping funnel, and the mixture was stirred at room temperature for 3 h. The reaction mixture was poured into 300 ml of water, and an organic layer was extracted with methylene chloride, dried with magnesium sulfate and distilled to remove methylene chloride. After that reduced pressure distillation was performed to obtain 6.0 g of methylmercapto-2-chlorocyclohexanone (78% yield; b.p. 48.5°-47.5° C./0.3 mmHg).

Aufarbeitung

  1. extractionan organic layer was extracted with methylene chloride
  2. dry with materialdried with magnesium sulfate
  3. distillationdistilled
  4. customto remove methylene chloride
  5. distillationAfter that reduced pressure distillation

Quellen und Nachweise

ORD-Eintrag
ord-009bcf70564a4317818b21a0e11ac4a2
Quelldatensatz
uspto-grants-1997_11
Patentnummer
US05691111

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