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

HRID 434112

반응식

HRID 434112 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 99207715-chloro-2-methylsulfanylindan-1-one수율 74%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4ef9d0c4a7454984acaefa558dbabf84
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06670401B2

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