HRID1599758

反应详情

EQUATION

反应方程式

HRID 1599758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

3-Amino-4-(2-hydroxy-2-methylpropylamino)quinoline (7.5 g, 32 mmol) was combined with methoxyacetic acid (7.5 mL, 97 mmol) and heated at about 170° C. for about 3 hours. The resulting solid residue was dissolved in ethyl acetate (150 mL). The ethyl acetate solution was extracted twice with 0.2N sodium hydroxide, washed with water, dried over magnesium sulfate, treated with activated charcoal and then concentrated to a volume of about 50 mL. Hexane was added to the ethyl acetate and the resulting precipitate was collected and dried to provide 0.9 g of the desired product as a crystalline solid, m.p. 145°-148° C. Analysis: Calculated: % C, 67.3; % H, 6.7; % N, 14.7; Found: % C, 67.2; % H, 6.6; % N, 14.6.

WORKUP

后处理

  1. extractionThe ethyl acetate solution was extracted twice with 0.2N sodium hydroxide
  2. washwashed with water
  3. dry with materialdried over magnesium sulfate
  4. additiontreated with activated charcoal
  5. concentrationconcentrated to a volume of about 50 mL
  6. additionHexane was added to the ethyl acetate
  7. customthe resulting precipitate was collected
  8. customdried