HRID1648306

反应详情

EQUATION

反应方程式

HRID 1648306 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydroxide (50 mL of 4.0 N, 0.20 mol) was added to a stirred solution of ethyl 3-(formylamino)-1,2,3,4-tetrahydro-2-oxo-3-quinolinecarboxylate (11.3 g, 0.043 mol) in methanol (250 mL). After 30 minutes, a white precipitate appeared and, after 45 minutes water (50 mL) was added to the reaction. After refluxing overnight, hydrochloric acid (50 mL of 4.0 N, 0.20 mol) was added and the solvents were removed under reduced pressure. The residual solid was refluxed in ethanol (200 mL) for 1 hour, filtered to remove salt, and cooled to afford 6.8 g of product, mp 197°-200° C. Anal. Calc'd for C10H10N2O2 : C, 63.15; H, 5.30; N, 14.73. Found: C, 63.03; H, 5.37; N, 14.71.

WORKUP

后处理

  1. waita white precipitate appeared and, after 45 minutes
  2. temperatureAfter refluxing overnight
  3. customthe solvents were removed under reduced pressure
  4. temperatureThe residual solid was refluxed in ethanol (200 mL) for 1 hour
  5. filtrationfiltered
  6. customto remove salt
  7. temperaturecooled