HRID1672313
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
2.3 g (11 mmol) of 6-fluoro-3-nitro-quinolin-4-ol (Example 19b) in 12 ml POCl3 are heated kept at 130° C. for 4 h. The reaction mixture is cooled to 0° C. and poured into ice-water. A precipitate is formed, which is filtered off and washed with water. The solid material is dissolved in CH2Cl2 and washed with 0.1N NaOH and water. After drying the organic phase over MgSO4, the solvent is evaporated to dryness. The residue is dissolved in a few ml of CH2Cl2 and hexane is added. The title compound precipitates and is filtered off. Drying is done at 60° C. (high-vacuum) overnight. NMR (DMSO-d6): 9.38/s (1H), 8.32/d×d (1H), 8.18/d×d (1H) and 8.02/d×t (1H); HPLC: tret=11.82 min (Grad 1).
WORKUP
后处理
- customA precipitate is formed
- filtrationwhich is filtered off
- washwashed with water
- dissolutionThe solid material is dissolved in CH2Cl2
- washwashed with 0.1N NaOH and water
- dry with materialAfter drying the organic phase over MgSO4
- customthe solvent is evaporated to dryness
- dissolutionThe residue is dissolved in a few ml of CH2Cl2 and hexane
- additionis added
- customThe title compound precipitates
- filtrationis filtered off
- customDrying
- customis done at 60° C.
- custom(high-vacuum) overnight
- customtret=11.82 min (Grad 1)