HRID2066450
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Oxalyl chloride (0.9 mL, 10 mmol) was added to a suspension of 4-bromo-1H-indole-2-carboxylic acid (2.1 g, 8.8 mmol) in DCM and the mixture was stirred for 2 h. The solution formed was added drop-wise to a stirring mixture of ammonia (37%, 50 mL) and ice (50 mL). The resulting mixture was allowed to stand for 3 days. The mixture was filtered and the filtrate extracted with EtOAc. The solid from the filtration was dissolved in EtOAc and the organic solutions were combined, dried (MgSO4) and then evaporated to afford the title compound as a brown solid (2.1 g, 100%).
WORKUP
后处理
- customThe solution formed
- additionwas added drop-wise
- waitto stand for 3 days
- filtrationThe mixture was filtered
- extractionthe filtrate extracted with EtOAc
- filtrationThe solid from the filtration
- dissolutionwas dissolved in EtOAc
- dry with materialdried (MgSO4)
- customevaporated