HRID2232206

反应详情

EQUATION

反应方程式

HRID 2232206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10 Grams of (2,3-dihydro-7-hydroxy-1-hydroxy-imino-4-methyl-1H-indene-6-yl)methylaminocarbonylmethylpyridinium chloride, 200 ml of acetic acid and 1.0 g of platinum oxide were subjected to catalytic hydrogenation under 3 atmospheric hydrogen gas pressure at room temperature for 8 hours. After the hydrogenation was completed, the catalyst was removed by filtration, and the filtrate was concentrated to dryness under a reduced pressure. The residue thus obtained was dissolved in 100 ml of methanol and under ice-cooled condition, a methanol solution saturated with hydrogen chloride gas was added thereto so as to adjust the pH of the solution to about pH 1, then the said solution was concentrated to dryness under a reduced pressure. The residue thus obtained was recrystallzed from ethanol-diethyl ether to obtain 4.8 g of 1-amino-2,3-dihydro-7-hydroxy-4-methyl-6-piperidinylacetylaminomethyl-1H-indene dihydrochloride. Colorless powdery crystals. Melting point: 146° C. (decomposed).

WORKUP

后处理

  1. customthe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated to dryness under a reduced pressure
  3. customThe residue thus obtained
  4. temperaturecooled condition
  5. concentrationthe said solution was concentrated to dryness under a reduced pressure
  6. customThe residue thus obtained