(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 → 乙酰丙酸

HRID 1528004

反应方程式

HRID 1528004 反应方程式
[OH:1][CH2:2][C:3]([C@H:5]([C@@H:7]([C@@H:9]([CH2:11][OH:12])[OH:10])O)[OH:6])=O.[CH3:13][OH:14].O.S(=O)(=O)(O)[OH:17]>CO.O>[OH:1][CH2:2][C:3]1[O:10][C:9]([CH:11]=[O:12])=[CH:7][CH:5]=1.[CH3:13][O:12][CH2:11][C:9]1[O:10][C:3]([CH:2]=[O:1])=[CH:5][CH:7]=1.[CH3:13][O:14][C:11](=[O:12])[CH2:9][CH2:7][C:5]([CH3:3])=[O:6].[C:11]([OH:12])(=[O:17])[CH2:9][CH2:7][C:5]([CH3:3])=[O:6]

参与物

9

反应物 4

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 1118四氧化硫HCID 5984D-(-)-Fructose4 次

产物 4

HCID 11579乙酰丙酸HCID 69354乙酰丙酸甲酯HCID 747115-甲氧基甲基-2-呋喃甲醛HCID 2373325-羟甲基糠醛

试剂、催化剂与溶剂 1

HCID 22242641Methanol--water (1/1)溶剂

反应条件

温度
60 °C

实验过程

An amount of 200 g fructose was added to 800 mL of a mixture of methanol and water (5 vol % water) that contained 55 mmol (5.4 gr) sulphuric acid. The admixture obtained was stirred at 60° C. until all solids were dissolved in about 2 hours. The solution was cooled down and a methanol/water mixture (5 vol % water) was added until 1.0 L of an homogeneous, clear solution was obtained. After dissolving the fructose the solution obtained was passed through a plug flow reactor that was heated at different temperatures, varying from 180 to 220° C. The residence time in the heated zone of the reactor was also varied and was set at 2 or 4 minutes. The pressure in this step was maintained at 65 bar. After having obtained a steady state condition in the reactor the product stream was analysed. The analysis determined the conversion (1 minus the number of moles of fructose in the product stream divided by the number of moles of fructose in the starting material, expressed in percent), and the yields for 5-hydroxymethylfurfural (HMF), 5-methoxymethylfurfural (“MMF”), methyllevulinate (“Me-Lev”) and levulinic acid (“LA”). The yield is expressed in percent and has been calculated as the number of moles of the compound in question divided by the initial amount of moles of fructose times 100. The results are shown in Table 3.

后处理

  1. customThe admixture obtained
  2. dissolutionwere dissolved in about 2 hours
  3. temperatureThe solution was cooled down
  4. customwas obtained
  5. customobtained
  6. customwas passed through a plug flow reactor
  7. temperaturethat was heated at different temperatures
  8. customvarying from 180 to 220° C
  9. customwas set at 2 or 4 minutes
  10. temperatureThe pressure in this step was maintained at 65 bar
  11. customAfter having obtained a steady state condition in the reactor the product stream

来源与证据

ORD记录
ord-090c1875a29d4f358de8445eccbde59d
来源数据集
uspto-grants-2015_07
专利号
US09090581B2

关联笔记

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