HRID1431298

反应详情

EQUATION

反应方程式

HRID 1431298 的结构方程式

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

  1. temperaturewas heated
  2. temperatureto reflux for 2 h
  3. additionThe reaction solution was poured into ice
  4. extractionThe aq. mixture was extracted with 2×75 mL DCM
  5. filtrationfiltered
  6. concentrationthe filtrate concentrated under reduced pressure
  7. customto afford a pale yellow solid, which