HRID1856504

反应详情

EQUATION

反应方程式

HRID 1856504 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 0.1 Mol of 4-nitro-3-methyl-2-butenol was added 0.1 Mol of melted p-chlorophenylisocyanate. The reaction mixture was allowed to stand at room temperature for several hours, before it was dissolved in hot benzene. After crystallizing overnight a solid by-product was filtered off and the benzene was evaporated. The residue was purified by dissolving in a hot hexane-benzene mixture, decanting, while hot, from an insoluble oil, followed by crystallization in a ice bath. The product was obtained as orange crystals, m.p. 79°-81°.

WORKUP

后处理

  1. waitto stand at room temperature for several hours, before it
  2. customAfter crystallizing overnight a solid by-product
  3. filtrationwas filtered off
  4. customthe benzene was evaporated
  5. customThe residue was purified
  6. dissolutionby dissolving in a hot hexane-benzene mixture
  7. customdecanting
  8. customwhile hot, from an insoluble oil, followed by crystallization in a ice bath
  9. customThe product was obtained as orange crystals, m.p. 79°-81°