HRID1801987

反应详情

EQUATION

反应方程式

HRID 1801987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Iodo-1-methyl-1H-benzo[d][1,3]oxazine-2,4-dione. To a stirred solution of 5-iodo-2-(methylamino)benzoic acid (10 g, 36 mmol), sodium carbonate (4 g, 36 mmol) and water (130 mL, 7218 mmol), cooled to 0° C., was slowly added, via addition funnel, a 2M phosgene (18 mL, 36 mmol) solution in toluene. After 2 hours, the precipitated product was isolated by filtration. The solids were washed with 100 mL of water, 150 mL of a 1:1 mixture of EtOH and ether, 100 mL of ether, and dried under vacuum to give the title compound.

WORKUP

后处理

  1. additionwas slowly added, via addition funnel
  2. customthe precipitated product was isolated by filtration
  3. washThe solids were washed with 100 mL of water, 150 mL of a 1:1 mixture of EtOH and ether, 100 mL of ether
  4. customdried under vacuum