反应 #1178470
ord-87cecb4c941d4d2a8bcb8345b41b0ae2
反应方程式
反应物
试剂
反应条件
后处理
- 1workup.STIRRINGthe reaction mixture was stirred for 3.5 hours
- 2workup.STIRRINGWhile the reaction mixture was stirred again under ice cooling
- 3workup.STIRRINGthe mixture was stirred for 20 minutes
- 4其他Precipitated insoluble matter was removed through separation by filtration
- 5浓缩the obtained mother liquor was concentrated under reduced pressure
实验过程
To an anhydrous tetrahydrofuran solution (100 mL) of lithium aluminum hydride (1.14 g, 29.93 mmol), a tetrahydrofuran solution (50 mL) of 1-benzhydrylazetidin-3-carboxylic acid methyl ester (Oakwood Products, Inc.: Code No. W07L) (2.00 g, 7.16 mmol) was added dropwise over 10 minutes under ice cooling and stirring, and the reaction mixture was stirred for 3.5 hours. While the reaction mixture was stirred again under ice cooling, water (1.14 mL), a 4N-aqueous solution of sodium hydroxide (1.14 mL) and water (4.50 mL) were added to the reaction liquor, and the mixture was stirred for 20 minutes. Precipitated insoluble matter was removed through separation by filtration, and the obtained mother liquor was concentrated under reduced pressure to obtain the title compound (1.97 g, over yield) as an oily matter.