反应 #342203

ord-807d2e2c31bd4949a3853874c391eff6

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction mixture was heated
  2. 2
    温度to reflux in a flask
  3. 3
    其他equipped with a Dean Stark trap and condensor
  4. 4
    温度After refluxing for 2.5 hours
  5. 5
    温度the reaction solution was cooled in an ice bath which
  6. 6
    其他resulted in the formation of a white precipitate
  7. 7
    其他The solid was isolated by filtration
  8. 8
    洗涤washed with 5% HCl (3×80 mL)

实验过程

To a mixture of phthalic anhydride (14.8 g, 100 mmole) and 4-aminobutyric acid (10.3 g, 100 mmole) in 150 mL of dry toluene was added triethylamine (1.3 mL, 9.3 mmole). The reaction mixture was heated to reflux in a flask equipped with a Dean Stark trap and condensor. After refluxing for 2.5 hours, the reaction solution was cooled in an ice bath which resulted in the formation of a white precipitate. The solid was isolated by filtration and washed with 5% HCl (3×80 mL) followed by cold water (2×70 mL). 4-Phthalimidobutyric acid was obtained as a white powder (16.8 g, 72%). m.p.: 118-118.6° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07875728B2uspto-grants-2011_01