HRID1393690

反应详情

EQUATION

反应方程式

HRID 1393690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2,3-Dihydro-1H-isoindole (543 mg) and 3-amino-3-methylbutanoic acid (700 mg) were dissolved in N,N-dimethylformamide (30 ml). N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (876 mg) and hydroxybenzotriazole (698 mg) were added thereto at 0° C., and then the mixture was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure, and water and ethyl acetate were added to the residue. The organic phase was separated, and the aqueous phase was adjusted to pH 9 by adding a saturated sodium bicarbonate solution, and then extracted with ethyl acetate. The extract was dried over sodium sulfate and concentrated under reduced pressure to give the title compound (0.60 g, Y.:60%) as a brown oily matter.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and water and ethyl acetate
  2. additionwere added to the residue
  3. customThe organic phase was separated
  4. additionby adding a saturated sodium bicarbonate solution
  5. extractionextracted with ethyl acetate
  6. dry with materialThe extract was dried over sodium sulfate
  7. concentrationconcentrated under reduced pressure