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[ CAS No. 139756-23-3 ] {[proInfo.proName]}

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Chemical Structure| 139756-23-3
Chemical Structure| 139756-23-3
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Product Details of [ 139756-23-3 ]

CAS No. :139756-23-3 MDL No. :MFCD21496447
Formula : C18H22N4O2 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W :326.39 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 139756-23-3 ]

* 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 [ 139756-23-3 ]

[ 139756-23-3 ] Synthesis Path-Downstream   1~3

  • 1
  • [ 139756-04-0 ]
  • [ 139756-23-3 ]
YieldReaction ConditionsOperation in experiment
96% With sodium hydroxide; In ethanol;Reflux; 34.4g (O.lmol) of starting material A was added in sequence. Ethanol 100mL, then add 8g (0.2mol) sodium hydroxide in batches, reflux reaction, TLC detects the disappearance of raw material spots. After the reaction is completed, it is cooled to room temperature, water is added to quench the reaction, and the pH is adjusted to neutrality with hydrochloric acid. White solid precipitated, suction filtered, The white solid was dried at 45 C to give 31.2 g (intermediate 1, yield 96%, purity 99.78%, maximum single impurity less than 0.10%).
59% With dihydrogen peroxide; potassium carbonate; In methanol; ethanol; dichloromethane; water; EXAMPLE 19 1-Methyl-5-(2-n-propoxyphenyl)-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one <strong>[139756-04-0]1-Methyl-4-(2-n-propoxybenzamido)-3-n-propylpyrazole-5-carboxamide</strong> (0.34 g, 0.99 mmol) was added to a stirred mixture of 30% hydrogen peroxide solution (1.0 ml), potassium carbonate (0.54 g, 3.92 mmol), water (10 ml) and ethanol (5 ml). The mixture was heated under reflux for 38 hours and then evaporated under vacuum. The residue was suspended in water (20 ml), then the mixture acidified with 2N hydrochloric acid and extracted with dichloromethane (3*20 ml). The extracts were combined, dried (Na2 SO4) and evaporated under vacuum. The resulting residue was chromatographed on silica gel (6 g), using a methanol in dichloromethane elution gradient (0.0-1.0%), to give an oil, successive trituration of which with ether gave the required product as a white solid (0.19 g, 59%), m.p. 111-114 C. Found: C,66.26; H,6.92; N,17.15. C18 H22 N4 O2 requires C,66.23; H,6.80; N,17.17%.
59% With dihydrogen peroxide; potassium carbonate; In methanol; ethanol; dichloromethane; water; PREPARATION 10 1-Methyl-5-(2-n-propoxyphenyl)-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-pyrimidin-7-one <strong>[139756-04-0]1-Methyl-4-(2-n-propoxybenzamido)-3-n-propylpyrazole-5-carboxamide</strong> (0.34 g, 0.99 mmol) was added to a stirred mixture of 30% hydrogen peroxide solution (1.0 ml), potassium carbonate (0.54 g, 3.92 mmol), water (10 ml) and ethanol (5ml). The mixture was heated under reflux for 38 hours and then evaporated under vacuum. The residue was suspended in water (20 ml), then the suspension acidified with 2N hydrochloric acid and extracted with dichloromethane (3*20 ml). The extracts were combined, dried (Na2 SO4) and evaporated under vacuum. The resulting residue was chromatographed on silica gel (6 g), using a methanol in dichloromethane elution gradient (0-1% methanol), to give an oil, successive trituration of which with ether gave the required product as a white solid (0.19 g, 59%), m.p. 111-114 C. Found: C,66.26; H,6.92; N,17.15. C18 H22 N4 O2 requires C,66.23; H,6.80; N, 17.17%
59% With dihydrogen peroxide; potassium carbonate; In methanol; ethanol; dichloromethane; water; EXAMPLE 113 1-Methyl-5-(2-n-propoxyphenyl)-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one <strong>[139756-04-0]1-Methyl-4-(2-n-propoxybenzamido)-3-n-propylpyrazole-5-carboxamide</strong> (0.34 g, 0.99 mmol) was added to a stirred mixture of 30% hydrogen peroxide solution (1.0 ml), potassium carbonate (0.54 g, 3.92 mmol), water (10 ml) and ethanol (5 ml). The mixture was heated under reflux for 38 hours and then evaporated under vacuum. The residue was suspended in water (20 ml), then the mixture acidified with 2N hydrochloric acid and extracted with dichloromethane (3*20 ml). The extracts are combined, dried (Na2SO4) and evaporated under vacuum. The resulting residue was chromatographed on silica gel (6 g), using a methanol in dichloromethane elution gradient (0.0-1.0%), to give an oil, successive trituration of which with ether gave the required product as a white solid (0.19 g, 59%), m.p. 111-114 C. Found: C, 66.26; H, 6.92; N, 17.15. C18H22N4O2 requires C, 66.23; H, 6.80; N, 17.17%.
With dihydrogen peroxide; sodium hydroxide; In ethanol; at 120℃; for 0.416667h;Microwave irradiation; 3) 1-methyl-3-propyl-5 - (2-propoxy-phenyl) - 1,6-dihydro -7H-pyrazolo-[ 4,3-d] pyrimidin-7-one preparation: heating 6mmol compound 1-methyl-3-propyl-4 - (2-propoxy benzamido- ) pyrazole-5-carboxamide dissolved in 40 ml volume ratio (20-80): 1 ethanol in a mixture with hydrogen peroxide, add 6mmol naoh, stirring to dissolve, microwave heating 120 C reaction 25 minutes, after the reaction of the organic solvent is removed by reduced pressure distillation, the residue is distilled water washes, ethyl acetate extraction, organic subtraction-pressure distillation to remove the solvent, dried to obtain 1-methyl-3-propyl-5 - (2-propoxy-phenyl) - 1,6-dihydro -7H-pyrazolo-[ 4,3-d] pyrimidin-7-one, yield 85-90%;

  • 2
  • [ 2100-31-4 ]
  • [ 139756-23-3 ]
  • 3
  • [ 139756-23-3 ]
  • [ 268203-93-6 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1: thionyl chloride; chlorosulfonic acid / 20 - 25 °C 2: 1 h / 10 - 20 °C
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