HRID366550

反应详情

EQUATION

反应方程式

HRID 366550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

2-Oxindole (82.9 9) was suspended in 630 mL of acetic acid with mechanical stirring and the mixture cooled to 10° C. in an ice water bath. Solid N-iodosuccinimide (175 g) was added in portions over 10 minutes. After the addition was complete the mixture was stirred for 1.0 hour at 10° C. The suspended solid which had always present became very thick at this time. The solid was collected by vacuum filtration, washed with 100 mL of 50% acetic acid in water and then with 200 mL of water and sucked dry for 20 minutes in the funnel. The product was dried under vacuum to give 93.5 g (36%) of 5-iodo-2-oxindole containing about 5% 2-oxindole by proton NMR.

WORKUP

后处理

  1. additionAfter the addition
  2. stirringwas stirred for 1.0 hour at 10° C
  3. filtrationThe solid was collected by vacuum filtration
  4. washwashed with 100 mL of 50% acetic acid in water
  5. dry with materialwith 200 mL of water and sucked dry for 20 minutes in the funnel
  6. customThe product was dried under vacuum