碘甲烷 → 2,2,5,5-四甲基-1,3-二噁烷-4,6-二酮

HRID 240297笔记

反应方程式

HRID 240297 反应方程式
[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[CH2:6][C:4](=O)O1.[C:11](=[O:14])([O-:13])[O-].[K+].[K+].[CH3:17]I>C(#N)C.ClCCl>[CH3:10][C:2]1([CH3:1])[O:13][C:11](=[O:14])[C:6]([CH3:17])([CH3:4])[C:7](=[O:8])[O:9]1

参与物

6

反应物 3

HCID 6328碘甲烷HCID 11430碳酸钾HCID 16249米氏酸

产物 1

HCID 3808172,2,5,5-四甲基-1,3-二噁烷-4,6-二酮

试剂、催化剂与溶剂 2

HCID 6342乙腈溶剂HCID 6344二氯甲烷溶剂

反应条件

温度
75 °C

实验过程

A mixture of Meldrum's acid (5.52 g, 38.3 mmol), potassium carbonate (26.5 g, 191 mmol) and methyl iodide (7.15 mL, 115 mmol) in acetonitrile (75 mL) was heated at 75° C. in a sealed tube for 7 hrs. The mixture was cooled to room temperature, diluted with dichloromethane (300 mL), filtered and the filtrate evaporated to dryness in vacuo. Ethyl acetate (75 mL), hexanes (75 mL) and water (50 mL) were added and phases were separated. The organic layer was washed with 10% aqueous solution of sodium thiosulfate (50 mL) and water (50 mL); dried over anhydrous magnesium sulfate and solvent removed in vacuo to give 2,2,5,5-tetramethyl-[1,3]dioxane-4,6-dione as white solid.

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationfiltered
  3. customthe filtrate evaporated to dryness in vacuo
  4. additionEthyl acetate (75 mL), hexanes (75 mL) and water (50 mL) were added
  5. customphases were separated
  6. washThe organic layer was washed with 10% aqueous solution of sodium thiosulfate (50 mL) and water (50 mL)
  7. dry with materialdried over anhydrous magnesium sulfate and solvent
  8. customremoved in vacuo

来源与证据

ORD记录
ord-e1085941cfd24ae9aaaf89254e77a40b
来源数据集
uspto-grants-2014_02
专利号
US08648041B2

反应笔记

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