HRID1431298
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 8-chloro-2,3-dimethylquinolin-4-ol (1.83 g, 8.81 mmol) in phosphorous oxychloride (10.00 mL) was heated to reflux for 2 h, after which time LC-MS indicated only product present. The reaction solution was poured into ice and adjusted to pH>10. The aq. mixture was extracted with 2×75 mL DCM. The combined organic extracts were stirred over anhydrous magnesium sulfate, filtered and the filtrate concentrated under reduced pressure to afford a pale yellow solid, which was not further purified. Mass Spectrum (ESI) m/e=226.0 (M+1).
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux for 2 h
- additionThe reaction solution was poured into ice
- extractionThe aq. mixture was extracted with 2×75 mL DCM
- filtrationfiltered
- concentrationthe filtrate concentrated under reduced pressure
- customto afford a pale yellow solid, which