反应 #487509

ord-3f0738e119114fdcbc6b23a076db3b5d

反应方程式

O=S(=O)(O)O
sulfuric acid
O=S(=O)(O)O
sulfuric acid
O=C1c2ccccc2C(=O)c2c1ccc(O)c2O
alizarin
O=C1c2ccccc2C(=O)c2c(O)c(O)cc(O)c21
purpurin

反应条件

温度
10°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他had been prepared
  2. 2
    温度cooling
  3. 3
    workup.ADDITIONwas added over 1 hour to a reaction liquid
  4. 4
    其他the reaction liquid
  5. 5
    洗涤being washed with 400 mL of water
  6. 6
    过滤filtered
  7. 7
    过滤The crystal collected by filtration
  8. 8
    洗涤was washed with 300 mL of methanol
  9. 9
    其他dried

实验过程

A suspension of 17.5 g of manganese dioxide/40 g of concentrated sulfuric acid, that had been prepared by putting 9.0 g of water and 130 g of 96% sulfuric acid into 30 g of alizarin (manufactured by Sigma-Aldrich Corporation), followed by ice-cooling, was added over 1 hour to a reaction liquid while maintaining it at 10° C. or lower. After 2 hours, the reaction liquid was poured into 1 L of water, with the inside of the container being washed with 400 mL of water, and filtered. The crystal collected by filtration was washed with 300 mL of methanol and dried to obtain 32.4 g of purpurin.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08741513B2uspto-grants-2014_06