反应 #2314292

ord-18f501d984b24e3083447518d18b89e1

反应方程式

C=CC=CCCCCC
isoprene
C=CC=CCCCCC
pentylbutadiene
C=COC(C)=O
vinyl acetate
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
CC(=O)OC1CC=C(C)CC1
4-Methyl-3-cyclohexenol acetate

溶剂

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.WAITto stand at 4° C. for a further 16 hours
  2. 2
    萃取The reaction mixtire is then sequentially extracted with two portions (150 mL each) of 1% hydrochloric acid solution, water (75 mL), and brine (75 mL)
  3. 3
    干燥It is dried over sodium sulfate
  4. 4
    过滤filtered through Celite
  5. 5
    浓缩concentrated in vacuo
  6. 6
    workup.DISTILLATIONThe product is distilled
  7. 7
    其他to give 30 g of clear, colorless liquid

实验过程

To a solution of vinyl acetate 4A (20 mL) in anhydrous toluene (220 mL) is added aluminum chloride (2.89 g). The flask is cooled to 0° C., and the isoprene 1C (R=methyl) (21.7 mL) is added dropwise. The reaction mixture is stirred 5 hours at 0° C., then allowed to stand at 4° C. for a further 16 hours. The reaction mixtire is then sequentially extracted with two portions (150 mL each) of 1% hydrochloric acid solution, water (75 mL), and brine (75 mL). It is dried over sodium sulfate, filtered through Celite, and concentrated in vacuo. The product is distilled to give 30 g of clear, colorless liquid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06413448B1uspto-grants-2002_07