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Chemical Structure| 7623-10-1 Chemical Structure| 7623-10-1

Structure of 7623-10-1

Chemical Structure| 7623-10-1

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Product Details of [ 7623-10-1 ]

CAS No. :7623-10-1
Formula : C4H6Cl2O
M.W : 141.00
SMILES Code : O=C(Cl)C(C)CCl

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Application In Synthesis of [ 7623-10-1 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 7623-10-1 ]

[ 7623-10-1 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 7623-10-1 ]
  • [ 496-11-7 ]
  • [ 202667-45-6 ]
YieldReaction ConditionsOperation in experiment
63.3% under the protection,AlCl3 (110 mmol, 14.61 g) was added to a 250 mL three-necked flask,After adding 130mLDichloromethane was stirred at -78 C, and indane (100 mmol, 11.82 g)With 2-methyl-3-chloropropionyl chloride(100 mmol, 12.82 g)Of methylene chloride solution,Reaction 24h,The reaction solution was slowly added to dilute hydrochloric acid to terminate the reaction,With saturated aqueous sodium carbonate solution, water,Saturated aqueous sodium chloride solution,Followed by extraction with 100 mL of dichloromethane,Combine organic phase,Dried over anhydrous magnesium sulfate for 2 h.Filtered, steamed and dried in vacuo to give 21.24 g of a white solid in 95.4% yield.The solid was slowly added to about 100 mL of concentrated sulfuric acid,Heated to 85 C, reflux.The reaction solution was slowly added to about 500 mL of ice water,Washed with saturated aqueous sodium carbonate solution to neutral, and filtered to give 14.83 g of terracotta solid, yield 83.4%.Ice water bath,The solid (79.6 mmol, 14.83 g) was dissolved in 100 mL of methanol,To this was slowly added sodium borohydride (160 mol, 6.05 g)Stirring reaction.Remove the methanol, add 100 mL of water, and use dilute hydrochloric acid to neutralize the pH.Extracted with 200 mL of dichloromethane, the combined organic phases were dried over anhydrous magnesium sulfate for 2 h.Filtered, steamed and dried in vacuo to give 12.83 g of a pale yellow solid in 85.2% yield.The solid (68 mmol, 12.83 g) was dissolved in about 150 mL of benzene,P-Toluenesulfonic acid (1.3 mmol, 0.25 g),Heated to 75 C and refluxed.Washed with saturated aqueous sodium carbonate solution to near neutral,The organic phase was dried over anhydrous magnesium sulfate for 2 h. The solid was removed by suction filtration, dried, dissolved with methylene chloride,Column chromatography was carried out using petroleum ether as eluent. To give 7.33 g of a pale yellow solid,Yield 63.3%
 

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