HRID54383
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To 5,6,7-trifluoro-1,4-dihydro-2,3-quinoxalinedione (93 mg, 0.43 mmol) is added concentrated sulfuric acid (0.5 mL). While the flask is an ice bath, KNO3 is slowly added, giving a brown mixture, which is stirred overnight. The reaction mixture, now dark red, is then added into ice water (5 mL), instantly giving an orange precipitate, which is collected by centrifugation. The powder was crystallized from EtOH (5 mL) and dried in vacuo to yield 24 mg (20%) of pale orange microcrystals. 1H NMR (DMSO-d6), 11.9 (br s, 1H), 12.6 (br s, 1H).
WORKUP
后处理
- customgiving a brown mixture, which
- custominstantly giving an orange precipitate, which
- customis collected by centrifugation
- customThe powder was crystallized from EtOH (5 mL)
- customdried in vacuo
- customto yield 24 mg (20%) of pale orange microcrystals