Alternatived Products of [ 91526-18-0 ] 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 : |
130.09
| Pubchem ID : | 10510878 |
Synonyms : | |
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.
- Downstream synthetic route of [ 91526-18-0 ]
- 1
- [ 37830-90-3 ]
- [ 91526-18-0 ]
Yield | Reaction Conditions | Operation in experiment |
| With selenium(IV) oxide; In 1,4-dioxane; | Example 26 Preparation of 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene A mixture of <strong>[37830-90-3]4,5-dimethyl-2-oxo-1,3-dioxole</strong>ne (1 mmol) and selenium dioxide (2.5 mmol) in dioxane was heated at reflux for 1 h. Evaporation, extraction and chromatography gave 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene as a yellow oil. TLC: Rf=0.5, 5percent MeOH-dichloromethane. |
| With selenium(IV) oxide; In 1,4-dioxane; | Example 17 Preparation of 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene A solution of <strong>[37830-90-3]4,5-dimethyl-2-oxo-1,3-dioxole</strong>ne (1 mmol) and selenium dioxide (2.5 mmol) in dioxane was heated at reflux for 1 h. Evaporation, extraction and chromatography gave 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene as a yellow oil. TLC: Rf=0.5, 5percent MeOH-dichloromethane. |
| With selenium(IV) oxide; In 1,4-dioxane; for 1h;Heating / reflux; | [01658] A solution of <strong>[37830-90-3]4,5-dimethyl-2-oxo-1,3-dioxole</strong>ne (1 mmole) and selenium dioxide (2.5 mmole) in dioxane was heated at reflux for 1 h. Evaporation, extraction and chromatography gave 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene as a yellow oil. TLC: RPf=0.5, 5percent MeOH-dichloromethane. [01659] A solution of 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene (1 mmole) in DMF was treated with tert-butyldimethylsilane (1.2 mmole) and imidazole (2.2 mmole) at 25 C. for 24 h. Extraction and chromatography gave 5-methyl-4-tert-butyldimethylsilyloxymethyl-2-oxo-1,3-dioxolene. [01660] A solution of 5-methyl-4-tert-butyldimethylsilyloxymethyl-2-oxo-1,3-dioxolene (1 mmole) and Lawesson's reagent (1.2 mmole) in toluene was heated to 120 C. for 12 h. Extraction and chromatography gave 5-methyl-4-tert-butyldimethylsilyloxymethyl-2-thio-1,3-dioxolene. [01661] A solution of 5-methyl-4-tert-butyldimethylsilyloxymethyl-2-thio-1,3-dioxolene in methanolic hydrogen chloride was stirred at 0 C. for 1 h and 25 C. for 12 h. Extraction and chromatography gave 5-methyl-4-hydroxymethyl-2-thio-1,3-dioxolene. |
- 2
- [ 150058-27-8 ]
- [ 91526-18-0 ]
- (5-methyl-2-oxo-1,3-dioxol-4-yl)methyl-2-ethoxy-1H-benzo[d]imidazol-7-carboxylate [ No CAS ]
Yield | Reaction Conditions | Operation in experiment |
91.6% | | The 45g2-ethoxy -1H-benzimidazole-7-carboxylic acid and 500 ml by adding dichloromethane for added to a reaction flask, stirring cooling to 20 °C the following, to-drop 50.7g triethylamine, the drop finishes, drop by adding 54.0g to toluene sulfonyl chloride and 100 ml dichloromethane mixed solution, drop Bi Yu 10-20 °C stirring reaction 3h, for 10-20 °C adding 39.7g4-hydroxymethyl-5-methyl -1,3-dioxol-2-one, the temperature rising to adding 30-40 °C stirring reaction, with used in HPLC. After the reaction is complete, cooling to 15-25°C, by adding 400 ml purified water stirring, layered, with 30g drying by anhydrous sodium sulfate. Decompression jeung dry dichloromethane, by adding 300 ml methyl tert-butyl ether refined, cooling to 0-5 °C stirring crystallization 3h, filtering, with 20 ml cool to 0-5 °C methyl tert-butyl ether washing, for 40-50 °C reduced-pressure drying to the job (5-methyl-2-oxo -1,3-dioxol-4-yl) methyl 2-ethoxy -1H-benzo[d] imidazol-7-carboxylic acid ester 63.6 g. The yield of 91.6percent, purity 98.1percent |