HRID1445712

反应详情

EQUATION

反应方程式

HRID 1445712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

L-Norvaline ethyl ester hydrochloride (50 gm) was dissolved in ethanol (600 ml). Sodium hydroxide (15.4 gm) dissolved in ethanol (500 ml) was added to the above at 10° C. and stirred for 30 minutes. Pyruvic acid (34.5 gm) solution in ethanol (200 ml) was then added to above reaction mass at 10° C. and stirred for 30 minutes. The reaction mass was then transferred to a hydrogenator along with 10% palladium on carbon (5 gm) and hydrogenated at 7 bar for 8 hours. The contents were filtered over celite and washed with ethanol (200 ml). The filtrate was concentrated completely under vacuum at about 50° C. Acetone (800 ml) was added to the residue and the contents refluxed for 1 hour and then cooled to room temperature and filtered to obtain the product (30 gm) as white crystals.

WORKUP

后处理

  1. additionwas added to the above at 10° C.
  2. stirringstirred for 30 minutes
  3. filtrationThe contents were filtered over celite
  4. washwashed with ethanol (200 ml)
  5. concentrationThe filtrate was concentrated completely under vacuum at about 50° C
  6. additionAcetone (800 ml) was added to the residue
  7. temperaturethe contents refluxed for 1 hour
  8. filtrationfiltered