반응 #311649

ord-07d8b452c2364852bfe5eaac08c6343c

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The methylene chloride was evaporated by means of steam
  2. 2
    온도after cooling to a melt cake that
  3. 3
    기타was isolated by decantation
  4. 4
    workup.ADDITIONadded
  5. 5
    여과The precipitate was filtered with suction
  6. 6
    세척washed with benzine (boiling range: 50°-75° C.)
  7. 7
    기타After being dried the precipitate
  8. 8
    workup.STIRRINGwas stirred with acetonitrile
  9. 9
    여과filtered with suction

실험 절차

Boron trifluoride was introduced with vigorous refluxing (bath temperature 50° C.) into a mixture of 138 g (1 mole) of 2,3-dimethylhydroquinone, 370 g (1.62 moles) of myristic acid and 700 ml of methylene chloride until saturation. After standing overnight the reaction mixture was decomposed by pouring into 3 l of a 10% by weight sodium acetate solution with stirring. The methylene chloride was evaporated by means of steam. The residual oily layer solidified after cooling to a melt cake that was isolated by decantation. It was melted up and added with stirring to 2 l of high-boiling benzine. The precipitate was filtered with suction and washed with benzine (boiling range: 50°-75° C.). After being dried the precipitate was stirred with acetonitrile and filtered with suction.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04232107uspto-grants-1980_11