反应 #2756

ord-c8bd279ef8414749819522d3b3ae0914

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONthe hot solution was introduced into the high pressure autoclave
  2. 2
    过滤The crystals were filtered off
  3. 3
    洗涤washed 3 times with cold 2,2,4-trimethylpentane
  4. 4
    其他The crystals were then dried in the drying cabinet at 50° C.

实验过程

Tri-o-thymotide (25 g) was dissolved in 2,2,4-trimethylpentane (50 ml) at 100° C. and the hot solution was introduced into the high pressure autoclave. Methyl bromide was added to the autoclave until a pressure of 200 bar was reached. The high pressure autoclave was then kept for 2 hours at 110° C. and the solution was then cooled down to room temperature within 5 days. The crystals were filtered off and washed 3 times with cold 2,2,4-trimethylpentane. The crystals were then dried in the drying cabinet at 50° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05730954uspto-grants-1998_03