反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto reflux
- additionwas added
- stirringStirring of the mixture
- waitwas continued for half an hour
- temperatureat reflux
- temperatureit was cooled down again to 33° C
- stirringafter continued stirring (overnight) the solid
- customwas isolated by filtration
- washwashed twice with 120 ml of methanol
- customAfter drying