HRID1154966

反应详情

EQUATION

反应方程式

HRID 1154966 的结构方程式

PROCEDURE

实验过程

To 1.20 g. (6.75 mmole) of (αS,5S)-α-amino-3-chloro-4,5-dihydro-5-isoxazol-acetic acid (AT-125), is added 20 ml. of 2 N sodium hydroxide and stirred at 25° for 36 hours. The solution is brought to ~3.5 pH with 6 N hydrochloric acid (dropwise addition) and then stored at -10° (freezer) overnight. The crystals are collected by filtration, washed twice with cold water, and then dried giving 720 mg. of trichloromic acid. The initial filtrate is lyophilized and the resulting powder is taken up in 4 ml. of water, filtered, and washed with two 4 ml. portions of cold water, and dried yielding an extra 160 mg. of tricholomic acid (total 80% yield).

WORKUP

后处理

  1. additiondropwise addition) and
  2. customthen stored at -10°
  3. custom(freezer) overnight
  4. filtrationThe crystals are collected by filtration
  5. washwashed twice with cold water
  6. customdried
  7. customgiving 720 mg
  8. filtrationof water, filtered
  9. washwashed with two 4 ml
  10. dry with materialportions of cold water, and dried
  11. customyielding an extra 160 mg