反应 #44951

ord-f9f37bcdc3464a7d9848ba524564d05b

反应条件

温度
5°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to obtain a solution
  2. 2
    其他The two phases were then separated
  3. 3
    workup.ADDITIONisobutyl methyl ketone (25 ml) was added to the aqueous phase
  4. 4
    workup.STIRRINGstirred for 10 minutes
  5. 5
    其他The two resulting phases were separated
  6. 6
    其他any traces of isobutyl methyl ketone was evaporated from the aqueous phase
  7. 7
    过滤The solid mupirocin calcium dihydrate was filtered
  8. 8
    洗涤washed with water (20 ml)
  9. 9
    其他dried under vacuum at 35° C. for 14 hours

实验过程

Pseudomonic acid (10.00 g, 20 mmole) was dissolved in isobutyl methyl ketone (100 ml) at 40° C. Calcium-2-ethyl-hexanoate (3.32 g, 10 mmole) was suspended in water (50 ml). (It is possible to obtain a solution by using a larger amount of water or an alcohol/water mixture). The solution of pseudomonic acid was added to the calcium-2-ethyl-hexanoate suspension, and the two phase system were stirred for 24 hours. The two phases were then separated, isobutyl methyl ketone (25 ml) was added to the aqueous phase, and stirred for 10 minutes. The two resulting phases were separated, and any traces of isobutyl methyl ketone was evaporated from the aqueous phase. The aqueous mupirocin calcium suspension was cooled in a refrigerator at 5° C. The solid mupirocin calcium dihydrate was filtered, washed with water (20 ml) and dried under vacuum at 35° C. for 14 hours. The mass of product was 7.95 grams. Assay 97.72%, water: 3.45%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07737177B2uspto-grants-2010_06