HRID359278

反应详情

EQUATION

反应方程式

HRID 359278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A reaction vessel was charged with 200 ml tetrahydrofuran and 28 g (100 mmol) of ethyl 2-[(1,1dimethylethyl)amino]-4-trifluoromethyl-5-oxazolecarboxylate (prepared by Example 6). With this mixture stirred at ambient temperature, 50% aqueous sodium hydroxide (16 g; 200 mmol) was added followed by 50 ml water as a rinse. The reaction mixture was stirred at ambient temperature for 16 hours. The mixture was then poured into 500 ml of 5% hydrochloric acid. After cooling with an ice bath, the mixture was filtered, washed with water, and then dried to yield 2.4 g of a white powder which was recrystallized from ethyl acetate to a crystalline product (m.p.=256°-258° C.) identified in Table I.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at ambient temperature for 16 hours
  2. temperatureAfter cooling with an ice bath
  3. filtrationthe mixture was filtered
  4. washwashed with water
  5. customdried