HRID1356608

反应详情

EQUATION

反应方程式

HRID 1356608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Racemic cis-1-amino-2-indanol (22.5 g, water wet, content 83.2%) was suspended with (R,R)-tartaric acid (65 g) in 120 ml of methanol of 60° C. After stirring for 1.5 hours at 60° C., 210 ml of methanol were added and the mixture was brought to reflux. At reflux a solution of racemic cis-1-amino-2-indanol (42.4 g, water wet, content 83.2%) in 120 ml of hot methanol was added. Stirring of the mixture was continued for half an hour at reflux and then it was cooled down again to 33° C. Methanol (10 ml) was added and after continued stirring (overnight) the solid was isolated by filtration and washed twice with 120 ml of methanol. After drying, 54.3 g of (1S,2R)-1-amino-2-indanol-(R,R)-tartrate methanol solvate were obtained with an e.e. of 97.5%. D[v, 0.9]=147.1 μm (measured with a Malvern 2600 apparatus).

WORKUP

后处理

  1. temperatureto reflux
  2. additionwas added
  3. stirringStirring of the mixture
  4. waitwas continued for half an hour
  5. temperatureat reflux
  6. temperatureit was cooled down again to 33° C
  7. stirringafter continued stirring (overnight) the solid
  8. customwas isolated by filtration
  9. washwashed twice with 120 ml of methanol
  10. customAfter drying