HRID462710

反应详情

EQUATION

反应方程式

HRID 462710 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

E-1. 1,2-Dihydro-5-methvl-2-oxo-1,6-naphthyridine-3-carbonitrile--A mixture containing 33.2 g of 5-acetyl-1,2-dihydro-6-(2-dimethylaminoethenyl)-2-oxo-3-pyridincarbonitrile, 32.1 g of formamidine acetate and 300 ml of dimethylformamide was heated in a oil bath at 120°-130° C. for 3 hours, the original yellow solid dissolving and dark solution resulting. The reaction mixture was evaporated to dryness and then treated with 400 ml of water followed by 30 ml of acetic acid. The resulting insoluble solid was collected, washed with water, air-dried, recrystallized from dimethylformamide and dried at 90° C. to yield 27.4 g of 1,2-dihydro-5-methyl-2-oxo-1,6-naphthyridine-3-carbonitrile as a compound containing 1/2 mole of dimethylformamide, m.p. 278°-280° C. with decomposition.

WORKUP

后处理

  1. temperaturewas heated in a oil bath at 120°-130° C. for 3 hours
  2. dissolutionthe original yellow solid dissolving
  3. customdark solution resulting
  4. customThe reaction mixture was evaporated to dryness
  5. additiontreated with 400 ml of water
  6. customThe resulting insoluble solid was collected
  7. washwashed with water
  8. customair-dried
  9. customrecrystallized from dimethylformamide
  10. customdried at 90° C.