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[ CAS No. 91526-18-0 ] {[proInfo.proName]}

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Product Details of [ 91526-18-0 ]

CAS No. :91526-18-0 MDL No. :MFCD12165896
Formula : C5H6O4 Boiling Point : -
Linear Structure Formula :- InChI Key :JEQSUJXHFAXJOW-UHFFFAOYSA-N
M.W : 130.10 Pubchem ID :10510878
Synonyms :

Safety of [ 91526-18-0 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P305+P351+P338 UN#:N/A
Hazard Statements:H302-H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 91526-18-0 ]

* 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.

  • Upstream synthesis route of [ 91526-18-0 ]
  • Downstream synthetic route of [ 91526-18-0 ]

[ 91526-18-0 ] Synthesis Path-Upstream   1~5

  • 1
  • [ 80841-78-7 ]
  • [ 91526-18-0 ]
YieldReaction ConditionsOperation in experiment
79%
Stage #1: With formic acid; triethylamine In acetonitrile at 10 - 65℃;
Stage #2: With hydrogenchloride In isopropyl alcoholReflux
Example 4APreparation of 4-hydroxymethyl-5-methyl-l, 3-dioxol-2-oneTo a solution of 4-chloromethyl-5methyl-l ,3-dioxol-2-one (50 g) in acetonitrile (500 ml), formic acid (45 g) was added at 20-25°C and the reaction mass cool to 10-15°C followed by addition of triethylamine (95 g). Reaction mass was heated to 60-65 °C and stirred at the same temperature for about 5-6 hrs. Reaction mass was cooled to 15-20°C, filtered and washed by acetonitrile. Filtrate was taken and acetonitrile was distilled out under vacuum to concentrate the solution. Reaction mass was cooled to 25-30°C and ethyl acetate and water was added, followed by stirring for about 15-20 minutes at 25- 30°C. Aqueous layer extracted with ethyl acetate and combined organic layer were washed with brine solution. Organic layer was separated and evaporated completely under vacuum below 35-40°C. To the oily mass, methanol was added and heated to reflux temperature. A solution of HC1 in isopropyl alcohol was added and the resulting solution was refluxed for about 60-75 mins. Reaction mass was cooled to 30-35°C. Distilled out the solvent completely to obtain title compound as oily mass. (Yield: 34.6 g; 79percent)
43%
Stage #1: With formic acid In acetonitrile at 20℃; for 0.0833333 h;
Stage #2: With triethylamine In acetonitrile at 0 - 60℃; for 8 h;
Stage #3: With hydrogenchloride In methanol at 20℃; for 2 h;
4- (chloromethyl)-5-methyl-1,3-dioxol-2-one (400mg, 2.7mmol) was dissolved in acetonitrile 10ml) was added dropwise formic acid (496mg, 10.8mmol ), then the mixture was stirred at room temperature for 5 minutes. The reaction mixture was cooled to 0 deg.] C, thereto was added triethylamine (0.8ml, 5.4mmol), and the mixture was stirred at 60 8 hours, and then water is introduced, and the mixture was extracted with ethyl acetate. The separated organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting residue was dissolved in methanol (10ml), and thereto was added concentrated hydrochloric acid (1ml), then, the mixture was stirred at room temperature for 2 hours. To the reaction mixture, saturated aqueous sodium bicarbonate is introduced, the mixture was extracted with ethyl acetate, then washed with saturated brine and the organic layer was separated, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate: n-hexane = 1: 2 (v / v)) for purification to prepare the title compound 150mg (43percent yield).
Reference: [1] Patent: WO2012/107814, 2012, A1, . Location in patent: Page/Page column 14-15
[2] Patent: CN105492423, 2016, A, . Location in patent: Paragraph 0741; 0742; 0743; 0744
[3] Patent: TW2016/2093, 2016, A, . Location in patent: Paragraph 0323
[4] Patent: US2016/194302, 2016, A1, . Location in patent: Paragraph 0413; 0414
  • 2
  • [ 37830-90-3 ]
  • [ 91526-18-0 ]
Reference: [1] Patent: US6054587, 2000, A,
[2] Patent: US6284748, 2001, B1,
[3] Patent: US6756360, 2004, B1, . Location in patent: Page column 162
  • 3
  • [ 80715-22-6 ]
  • [ 91526-18-0 ]
Reference: [1] Patent: US5416208, 1995, A,
  • 4
  • [ 91526-17-9 ]
  • [ 91526-18-0 ]
Reference: [1] Synthetic Communications, 1992, vol. 22, # 9, p. 1277 - 1282
[2] Synthetic Communications, 1995, vol. 25, # 23, p. 3875 - 3881
  • 5
  • [ 80715-22-6 ]
  • [ 91526-18-0 ]
Reference: [1] Synthetic Communications, 1995, vol. 25, # 23, p. 3875 - 3881
[2] Synthetic Communications, 1992, vol. 22, # 9, p. 1277 - 1282
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[ 91526-18-0 ]

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