HRID1739110
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
PROCEDURE
实验过程
8.1 g of triethylamine and then 4.9 g of dimethylamine hydrochloride are added to a solution of 6.11 g of the compound obtained in step A of PREPARATION 1.21 in 20 ml of DCM and 20 ml of DMF. The mixture is cooled in an ice bath, 9.73 g of BOP are added and the mixture is left stirring for 3 hours while allowing the temperature to rise to RT. The mixture is concentrated under vacuum, the residue is extracted with ether, the organic phase is washed with water, with a pH 2 buffer solution, with 10% NaOH solution, with water and with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. 6.45 g of the expected product are obtained.
WORKUP
后处理
- temperatureThe mixture is cooled in an ice bath
- waitthe mixture is left
- customto rise to RT
- concentrationThe mixture is concentrated under vacuum
- extractionthe residue is extracted with ether
- washthe organic phase is washed with water, with a pH 2 buffer solution, with 10% NaOH solution, with water and with saturated NaCl solution
- dry with materialdried over MgSO4
- customthe solvent is evaporated off under vacuum