HRID2061864

反应详情

EQUATION

反应方程式

HRID 2061864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 1-(1,3-dimethoxypropan-2-yl)-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylate (Intermediate 22, 270 mg, 0.60 mmol) was dissolved in tetrahydrofuran (20 mL) and water (5 mL). Lithium hydroxide (56 mg, 2.42 mmol) was added and the mixture was stirred for 10 min at room temperature. The reaction mixture was then refluxed at 80° C. for 1 h. The reaction mixture was concentrated under reduced pressure and water (10 mL) was added. The pH was adjusted to 2 with hydrochloric acid (2N) and the solid that precipitated was collected by filtration and dried to afford 185 mg (75%) of 1-(1,3-dimethoxypropan -2-yl)-6-iodo-4-oxo-1,4-dihydroquinoline-3-carboxylic acid.

WORKUP

后处理

  1. temperatureThe reaction mixture was then refluxed at 80° C. for 1 h
  2. concentrationThe reaction mixture was concentrated under reduced pressure and water (10 mL)
  3. additionwas added
  4. customthe solid that precipitated
  5. filtrationwas collected by filtration
  6. customdried