HRID1258677

反应详情

EQUATION

反应方程式

HRID 1258677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

DIC (130 μL, 0.8 mmol) was added to N-(4-chloro-3-{3-[2-methylamino-5-(4-trifluoromethyl-piperidin-1-yl)-phenyl]-thioureido}-benzyl)-2,2-dimethyl-propionamide (180 mg, 0.3 mmol) in MeCN. The reaction mixture was heated at 60° C.-80° C. for one week (additional DIC (2.5 ml) was added). The mixture was cooled to rt and concentrated. The residue was treated with MeCN, filtered and washed. The filtercake was diluted with dioxane and HCOOH and lyophilized to give the title compound.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated at 60° C.-80° C. for one week
  2. concentrationconcentrated
  3. additionThe residue was treated with MeCN
  4. filtrationfiltered
  5. washwashed
  6. additionThe filtercake was diluted with dioxane and HCOOH