HRID1955049

反应详情

EQUATION

反应方程式

HRID 1955049 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.98 g of triethylamine are added to a solution of 1.5 g of the compound obtained in the preceding stage in 5 ml of DCM and 5 ml of DMF, followed by 0.49 g of methylamine hydrochloride. The mixture is cooled on an ice bath, 2.39 g of BOP are added and the mixture is kept stirring for 24 hours while allowing the temperature to rise to RT. The reaction mixture is concentrated under vacuum, the residue extracted with ether, washed with water, with a buffer solution pH=2, with water, with a 10% solution of NaOH, with water, with a saturated solution of NaCl, dried over MgSO4 and evaporated under vacuum. 1.4 g of the expected product are obtained.

WORKUP

后处理

  1. temperatureThe mixture is cooled on an ice bath
  2. customto rise to RT
  3. concentrationThe reaction mixture is concentrated under vacuum
  4. extractionthe residue extracted with ether
  5. washwashed with water, with a buffer solution pH=2, with water, with a 10% solution of NaOH, with water, with a saturated solution of NaCl
  6. dry with materialdried over MgSO4
  7. customevaporated under vacuum