Sodium methanethiolate → 5-Chloro-2-methylsulfanylindan-1-one

HRID 896634ノート

反応式

HRID 896634 の反応式
Br[CH:2]1[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([Cl:11])[CH:8]=2)[C:3]1=[O:12].[CH3:13][S-:14].[Na+]>C(O)C>[Cl:11][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[C:3](=[O:12])[CH:2]([S:14][CH3:13])[CH2:10]2

参加物

4

反応物 2

HCID 4378561Sodium methanethiolateHCID 113340692-Bromo-5-chloro-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 99207715-Chloro-2-methylsulfanylindan-1-one収率 74%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.98 g (4 mmol) of 2-bromo-5-chloroindan-1-one and 0.42 g (6 mmol) of sodium thiomethoxide are suspended in 5 ml of ethanol, treated in an ultrasonic bath for 30 minutes and then stirred at room temperature for 90 minutes. The reaction mixture is concentrated under reduced pressure and chromatographed on silica gel using toluene/ethyl acetate 10/1. The eluates are concentrated under reduced pressure, giving 0.63 g of 5-chloro-2-methylsulfanylindan-1-one of melting point 90° C.

後処理

  1. additiontreated in an ultrasonic bath for 30 minutes
  2. concentrationThe reaction mixture is concentrated under reduced pressure
  3. customchromatographed on silica gel
  4. concentrationThe eluates are concentrated under reduced pressure

出典と根拠

ORDレコード
ord-0b4922af2afc4dfeadd571f416fb2abc
出典データセット
uspto-grants-2005_07
特許番号
US06919380B2

反応ノート

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