Water → 3,5-Dimethylthioanisole

HRID 130632

반응식

HRID 130632 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([SH:9])[CH:5]=[C:6]([CH3:8])[CH:7]=1.[C:10](=O)([O-])[O-].[K+].[K+].IC.O>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.CS(C)=O>[CH3:8][C:6]1[CH:5]=[C:4]([S:9][CH3:10])[CH:3]=[C:2]([CH3:1])[CH:7]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 1175483,5-Dimethylbenzenethiol

생성물 1

HCID 27586623,5-Dimethylthioanisole수율 88%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 679Dimethyl Sulfoxide용매

실험 절차

10.0 g (0.072 mol) of 3,5-dimethylbenzenethiol, 9.95 g (0.072 mol) of potassium carbonate and 0.46 g (1.4 mmol) of tetrabutylammonium bromide are suspended in 20 ml of dimethylsulfoxide under argon. Iodomethane (10.2 g, 0.072 mol) is added dropwise, and the mixture is stirred 16 h at ambient temperature. After pouring the mixture into water, the product is extracted with ether, washed with water, dried over sodium sulfate and concentrated in vacuo. The crude product 9.6 g (0.063 mol; 88%) is obtained as a slightly yellow oil, and is used for the next step without further purification.

후처리

  1. extractionthe product is extracted with ether
  2. washwashed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5d140823334b42bab843a470f385b15a
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07381842B2

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