反应 #985277

ord-44402c4e74054f17a07ff98eb19718e1

溶剂

反应条件

温度
5°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGstirred for one hour
  2. 2
    其他the resulting precipitated crystal
  3. 3
    过滤was filtered
  4. 4
    其他dried under reduced pressure

实验过程

p-Bromo-β-phenylalanine (10.0 g, 41 mmol) was mixed with 40 ml of water and adjusted to pH 14 with 25% sodium hydroxide aqueous solution. After being cooled to 5° C., 8.5 ml of acetic anhydride (90 mmol) and 25% sodium hydroxide aqueous solution were simultaneously dropped into the mixture to keep it at a pH range of 11.5˜12 and the resulting mixture was stirred for 3 hours at a room temperature. After the mixture was adjusted to pH 2 with conc. HCl and stirred for one hour, the resulting precipitated crystal was filtered and dried under reduced pressure to give quantitatively 12.0 g of acetyl-p-bromo-β-phenylalanine.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07351571B2uspto-grants-2008_04