反応 #345559

ord-fdd9448f249e477f8a46fab5d3f7a11d

反応方程式

CCCC[N+](CCCC)(CCCC)CCCC.[OH-]
tetrabutylammonium hydroxide
COC(=O)Cc1ccccc1
Methylphenylacetate
CCCC[N+](CCCC)(CCCC)CCCC.COC(=O)Cc1ccccc1
tetra-n-butyl ammonium methylphenylacetate

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated to +75° C. to +85° C
  2. 2
    workup.DISTILLATIONSimultaneously an azeotrope of toluene-water was distilled out slowly over a period of 3 hours
  3. 3
    workup.DISTILLATIONAfter all toluene had distilled over, the flask
  4. 4
    その他A solid product separated out
  5. 5
    洗浄which was repeatedly washed with dry hexane

実験手順

In a similar apparatus as described in example 2, 7.7 mmoles of tetrabutylammonium hydroxide (20% solution in toluene/methanol) in 40 ml of dry toluene was taken and heated to +75° C. to +85° C. Methylphenylacetate (9.0 mmoles) was slowly added. Simultaneously an azeotrope of toluene-water was distilled out slowly over a period of 3 hours. After all toluene had distilled over, the flask was cooled to room temperature slowly. A solid product separated out, which was repeatedly washed with dry hexane. The initiator (tetra-n-butyl ammonium methylphenylacetate) thus formed was dried in vacuum and stored at room temperature under nitrogen or argon.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05266702uspto-grants-1993_11