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Chemical Structure| 6279-86-3 Chemical Structure| 6279-86-3

Structure of 6279-86-3

Chemical Structure| 6279-86-3

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Product Details of [ 6279-86-3 ]

CAS No. :6279-86-3
Formula : C10H16O6
M.W : 232.23
SMILES Code : O=C(C(C(OCC)=O)C(OCC)=O)OCC
MDL No. :MFCD00009150
InChI Key :AGZPNUZBDCYTBB-UHFFFAOYSA-N
Pubchem ID :80471

Safety of [ 6279-86-3 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H315-H319-H335
Precautionary Statements:P261-P305+P351+P338

Application In Synthesis of [ 6279-86-3 ]

* 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 [ 6279-86-3 ]

[ 6279-86-3 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 6279-86-3 ]
  • [ 873-95-0 ]
  • [ 1332486-06-2 ]
YieldReaction ConditionsOperation in experiment
54% With sulfolane; at 150℃; for 5h; Ethyl 2,4-dihydroxy-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydroquinoline-3-carboxylate 150 g 3-amino-5,5-dimethyl-2-cyclohexen-1 -one and 250 ml 2-ethoxycarbonyl-malonic acid diethyl ester in 100 ml sulfolane are heated to 150 C. Volatiles are continuously distilled of at 100 mbar. After 5 h the reaction mixture is cooled to 100 C and treated with 70 ml dioxane. Then the reaction mixture is cooled to 50 C and treated with 500 ml methyl tert-butyl ether. The mixture is stirred at room temperature for 15 h and then the precipitate is collected by filtration and dried at 70 C. Yield: 163 g (54 % of theory) Mass spectrometry (ESI+): m/z = 280 [M+H]+ Rf-value: 0.24 (silica gel, dichloromethane/methanol 20:1 )
54% In sulfolane; at 150℃; under 75.0075 Torr; for 5h; 150 g <strong>[873-95-0]3-amino-5,5-dimethyl-2-cyclohexen-1-one</strong> and 250 ml 2-ethoxycarbonyl-malonic acid diethyl ester in 100 ml sulfolane are heated to 150 C. Volatiles are continuously distilled of at 100 mbar. After 5 h the reaction mixture is cooled to 100 C. and treated with 70 ml dioxane. Then the reaction mixture is cooled to 50 C. and treated with 500 ml methyl tert-butyl ether. The mixture is stirred at room temperature for 15 h and then the precipitate is collected by filtration and dried at 70 C. [0229] Yield: 163 g (54% of theory) [0230] Mass spectrometry (ESI+): m/z=280 [M+H]+ [0231] Rf-value: 0.24 (silica gel, dichloromethane/methanol 20:1)
49% at 210℃; for 0.166667h; Example IEthyl 2,4-dihvdroxy-7,7-dimethyl-5-oxo-5,6,7,8-tetrahvdroquinoline-3-carboxylate10 g 3-Amino-5,5-dimethyl-2-cyclohexen-1 -one and 25 g 2-Ethoxycarbonyl-malonic acid diethyl ester are combined and heated for 10 minutes at 210C (bath temperature).Thereafter the mixture is cooled to room temperature and triturated with diethylether. The crystalline precipitate is collected by filtration and dried in vacuo.Yield: 9,9 g (49 % of theory)Mass spectrometry (ESI+): m/z = 280 [M+H]+ Rf-value: 0,45 (silica gel, dichloromethane/methanol 9:1 )
49% at 210℃; for 0.166667h; 10 g 3-Amino-5,5-dimethyl-2-cyclohexen-1-one and 25 g 2-Ethoxycarbonyl-malonic acid diethyl ester are combined and heated for 10 minutes at 210 C. (bath temperature). Thereafter the mixture is cooled to room temperature and triturated with diethylether. The crystalline precipitate is collected by filtration and dried in vacuo.Yield: 9.9 g (49% of theory)Mass spectrometry (ESI+): m/z=280 [M+H]+ Rf-value: 0.45 (silica gel, dichloromethane/methanol 9:1)
49% at 210℃; for 0.166667h; Example IEthyl 2,4-dihvdroxy-7,7-dimethyl-5-oxo-5,6,7,8-tetrahvdroquinoline-3-carboxylate10 g 3-Amino-5,5-dimethyl-2-cyclohexen-1-one and 25 g 2-Ethoxycarbonyl-malonic acid diethyl ester are combined and heated for 10 minutes at 210C (bath temperature).Thereafter the mixture is cooled to room temperature and triturated with diethylether. The crystalline precipitate is collected by filtration and dried in vacuo.Yield: 9,9 g (49 % of theory)Mass spectrometry (ESI+): m/z = 280 [M+H]+ Rf-value: 0,45 (silica gel, dichloromethane/methanol 9: 1)
49% for 0.166667h;Heating; 10 g 3-Amino-5,5-dimethyl-2-cyclohexen-1-one and 25 g 2-Ethoxycarbonyl-malonic acid diethyl ester are combined and heated for 10 minutes at 210 C. (bath temperature). Thereafter the mixture is cooled to room temperature and triturated with diethylether. The crystalline precipitate is collected by filtration and dried in vacuo.[0523]Yield: 9.9 g (49% of theory)[0524]Mass spectrometry (ESI+): m/z=280 [M+H]+[0525]Rf-value: 0.45 (silica gel, dichloromethane/methanol 9:1)

 

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