HRID26483

反应详情

EQUATION

反应方程式

HRID 26483 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(N-butylamino)-4-methyloxazole (106.7 g., 0.69 m.) and triethylamine (110 g., 0.77 m.) was stirred together in dry benzene (1500 c.c.) during the addition of isobutyrylchloride (81.0 g., 0.76 m.). The mixture was stirred at room temperature for 15 hours and then water (1 litre) was added. After stirring for a further hour the organic phase was separated, and the aqueous phase extracted twice in ether. The combined extract was washed successively with 2N hydrochloric acid (2 × 500 c.c.), 10% sodium carbonate solution (2 × 500 c.c.), and saturated brine (2 × 500 c.c.). Evaporation of the dried organic phase gave an oil, which was distilled to give 2-(N-butylisobutyramido)-4-methyloxazole, (118 g., 80%), b.p. 75-76° C./0.15 mm., which existed as an oil at room temperature but crystallised on cooling to 0° C.

WORKUP

后处理

  1. stirringAfter stirring for a further hour the organic phase
  2. customwas separated
  3. extractionthe aqueous phase extracted twice in ether
  4. extractionThe combined extract
  5. washwas washed successively with 2N hydrochloric acid (2 × 500 c.c.), 10% sodium carbonate solution (2 × 500 c.c.), and saturated brine (2 × 500 c.c.)
  6. customEvaporation of the dried organic phase
  7. customgave an oil, which
  8. distillationwas distilled