HRID1801276

反应详情

EQUATION

反应方程式

HRID 1801276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 2-(4-chloro-3-isobutyramidophenyl)-3,3-dimethyl-1,2,3,4-tetrahydroquinoline-6-carboxylate (216 mg, 0.52 mmol) in methanol (8 mL) and 4.2 mL of aqueous solution of sodium hydroxide (1 M, 4.2 mmol) was stirred at reflux for 2 h. Thin layer chromatography indicated that the starting material was consumed completely. Methanol was removed under reduced pressure and the residue was acidified to pH=6 with 1 M hydrochloric acid solution. The precipitated white solid were collected by filtration and dissolved in Ethyl acetate, dried over anhydrous sodium sulfate. The solvent was removed in vacuo to afford 120 mg of 2-(4-chloro-3-isobutyramidophenyl)-3,3-dimethyl-1,2,3,4-tetrahydroquinoline-6-carboxylic acid as a white solid. LC-MS (M+1)=383.

WORKUP

后处理

  1. temperatureat reflux for 2 h
  2. customwas consumed completely
  3. customMethanol was removed under reduced pressure
  4. filtrationThe precipitated white solid were collected by filtration
  5. dissolutiondissolved in Ethyl acetate
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was removed in vacuo