Potassium Hydroxide → HCID 6476762、化合物

HRID 1195147ノート

反応式

HRID 1195147 の反応式
[CH3:1]/[C:2](/[CH2:6][CH2:7][CH:8]=[C:9]([CH3:11])[CH3:10])=[CH:3]\[CH2:4][SH:5].[OH-].[K+].Cl[CH:15]([C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=1[Cl:29])[CH2:16][N:17]1[CH:21]=[CH:20][N:19]=[CH:18]1>CO.C(O)C>[Cl:29][C:23]1[CH:24]=[C:25]([Cl:28])[CH:26]=[CH:27][C:22]=1[CH:15]([S:5][CH2:4]/[CH:3]=[C:2](\[CH3:1])/[CH2:6][CH2:7][CH:8]=[C:9]([CH3:11])[CH3:10])[CH2:16][N:17]1[CH:21]=[CH:20][N:19]=[CH:18]1

参加物

6

反応物 3

HCID 14797Potassium HydroxideHCID 6365572(E)-3,7-Dimethylocta-2,6-diene-1-thiolHCID 124607821-[2-Chloro-2-(2,4-dichlorophenyl)ethyl]-1H-imidazole

生成物 1

HCID 6476762HCID 6476762、化合物収率 54.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

To a stirred solution of (E)-3,7-dimethylocta-2,6-dienylmercaptan (1.00 g=5.9 mmol) in methanol (40 ml) was added potassium hydroxide (0.33 g=5.8 mmol) and 1-chloro-1-(2,4-dichlorophenyl)-2-(1H-imidazole-1-yl)ethane (1.62 g=5.9 mmol) in ethanol at room temperature, and then the reaction mixture was refluxed for 90 minutes. After cooling, the methanol was evaporated, and then the residue was diluted with chloroform. The chloroform layer was washed with water, followed by drying over anhydrous sodium sulfate. Concentration followed by column chromatography on silica gel (ethyl acetate:hexane=2:3) gave 1.32 g of Compound 10 as a colorless oil.

後処理

  1. temperaturethe reaction mixture was refluxed for 90 minutes
  2. temperatureAfter cooling
  3. customthe methanol was evaporated
  4. additionthe residue was diluted with chloroform
  5. washThe chloroform layer was washed with water
  6. dry with materialby drying over anhydrous sodium sulfate
  7. concentrationConcentration

出典と根拠

ORDレコード
ord-10baf165870b4d5da61e6c5298cf9bdb
出典データセット
uspto-grants-1992_05
特許番号
US05110826

反応ノート

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