Methanethiol → Methylmercapto-2-chlorocyclohexanone

HRID 2294766ノート

反応式

HRID 2294766 の反応式
[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]

参加物

6

反応物 4

HCID 878MethanethiolHCID 962WaterHCID 132032-ChlorocyclohexanoneHCID 5360545Sodium

生成物 1

HCID 54407380Methylmercapto-2-chlorocyclohexanone収率 78%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-009bcf70564a4317818b21a0e11ac4a2
出典データセット
uspto-grants-1997_11
特許番号
US05691111

反応ノート

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