反应 #2507840

ord-db3db0cadda847e3be84a6ece7695dfb

反应方程式

Brc1ccccc1
bromobenzene
CC(C)(Cl)CCC(C)(C)Cl
2,5-dichloro-2,5-dimethyl hexane
[Al+3].[Cl-].[Cl-].[Cl-]
Aluminum chloride
CC1(C)CCC(C)(C)c2cc(Br)ccc21
6-bromo-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A 200 ml round-bottomed flask equipped with a stir bar and a reflux condenser
  2. 2
    温度until spontaneous reflux subsides
  3. 3
    其他the layers were separated
  4. 4
    萃取The aqueous layer was extracted with EtOAc (5×20 ml)
  5. 5
    洗涤The combined organic layer was washed with water and brine
  6. 6
    干燥dried over sodium sulfate
  7. 7
    过滤filtered
  8. 8
    浓缩concentrated

实验过程

A 200 ml round-bottomed flask equipped with a stir bar and a reflux condenser was charged with a solution of bromobenzene (109 mmol, 17 ml) and 2,5-dichloro-2,5-dimethyl hexane (10 grams, 54.6 mmol) in dichloromethane (30 ml). Aluminum chloride (1.45 grams, 10.9 mmol) was added to the solution slowly, until spontaneous reflux subsides. After stirring for 10-15 minutes at room temperature, the reaction was poured into ice water (30 ml) and the layers were separated. The aqueous layer was extracted with EtOAc (5×20 ml). The combined organic layer was washed with water and brine, dried over sodium sulfate, filtered, and concentrated, to yield a 6-bromo-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07955852B2uspto-grants-2011_06