Methanethiol → Methylmercapto-2-chlorocyclohexanone

HRID 2294766노트

반응식

HRID 2294766 반응식
[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]

참가 물질

6

반응물 4

HCID 878MethanethiolHCID 962WaterHCID 132032-ChlorocyclohexanoneHCID 5360545Sodium

생성물 1

HCID 54407380Methylmercapto-2-chlorocyclohexanone수율 78%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-009bcf70564a4317818b21a0e11ac4a2
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05691111

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