反应 #1726708

ord-6e8ae098219249df9b35011e0df6ad9e

反应方程式

O
water
O=C(CBr)c1ccccc1
2-bromoacetophenone
O=C1NC(=O)c2ccccc21.[K]
potassium phthalimide
O=C(CN1C(=O)c2ccccc2C1=O)c1ccccc1
2-phthalimido-acetophenone
收率 86.0%

溶剂

反应条件

温度
40°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with chloroform (300 ml
  2. 2
    洗涤The combined organic phases were washed with sodium hydroxide (200 ml, 0.2 N), water (2×100 ml) and brine (100 ml)
  3. 3
    干燥dried over magnesium sulfate
  4. 4
    浓缩concentrated in vacuo
  5. 5
    过滤recovered by filtration
  6. 6
    洗涤washed with ether (100 ml)
  7. 7
    其他dried in vacuo

实验过程

A solution of 2-bromoacetophenone (30.0 g, 151 mmol) in DMF (120 ml) was treated with potassium phthalimide (30.8 g, 166 mmol) portionwise at ambient temperature, and then heated to 40° C. for 3.5 hr. The cooled mixture was poured into water (600 ml) and extracted with chloroform (300 ml then 100 ml). The combined organic phases were washed with sodium hydroxide (200 ml, 0.2 N), water (2×100 ml) and brine (100 ml), dried over magnesium sulfate and concentrated in vacuo. The resulting cream solid was suspended in ether (100 ml), recovered by filtration, washed with ether (100 ml) and dried in vacuo to yield pure 2-phthalimido-acetophenone as a white solid (34.3 g, 86%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08110568B2uspto-grants-2012_02