HRID279926

反应详情

EQUATION

反应方程式

HRID 279926 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
4 °C

PROCEDURE

实验过程

A solution of 20 g of glucosamine hydrochloride, 20 ml of glacial acetic acid, 80 ml of water and 9.1 ml of phenylhydrazine was heated on a steam bath for one hour, then cooled and filtered. The filtrate was hydrogenated in a Parr apparatus with Raney nickel catalyst until the uptake of hydrogen ceased. This mixture was then filtered, the filtrate was treated with activated charcoal and refiltered through diatomaceous earth, giving a green solution. A 6.31 ml portion of this green solution was treated with 0.24 g of sodium bicarbonate and a suspension of 1.66 g of potassium tetrachloroplatinate in 8 ml of water. The resulting reddish brown solution was stirred overnight, then cooled to 4° C. for 3 hours and the resulting solid collected. A 100 mg portion of this solid was stirred with 15 ml of hot water and then filtered through diatomaceous earth. The filtrate was cooled giving a solid which was collected, giving 90 mg of 1,2-diamino-1,2-dideoxy-D-glucitol, compound with platinum chloride (1:1) as yellow grains, mp 265° C. (dec.).

WORKUP

后处理

  1. temperaturecooled
  2. filtrationfiltered
  3. filtrationThis mixture was then filtered
  4. additionthe filtrate was treated with activated charcoal
  5. customgiving a green solution
  6. customthe resulting solid collected
  7. stirringA 100 mg portion of this solid was stirred with 15 ml of hot water
  8. filtrationfiltered through diatomaceous earth
  9. temperatureThe filtrate was cooled
  10. customgiving a solid which
  11. customwas collected