HRID2397540

反应详情

EQUATION

反应方程式

HRID 2397540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

At 0° a solution of 16.0 g of methyl chloroformate in THF was added dropwise to a solution of the sodium derivative of 32.7 g of methyl nitro(tetrahydro-2H-1,3-thiazin-2-ylidene)acetate (3A; Example 2, Ser. No. 554,371) in THF. The stirred solution was then allowed to warm to room temperature and stirred overnight. The solvent was evaporated under reduced pressure and the residue was poured into ether. The ether phase was washed with water, dried (MgSO4) and the solvent evaporated under reduced pressure. The resulting oil was mixed with pentane to give 3, as yellow crystals, m.p.: 71°-2°.

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. additionthe residue was poured into ether
  3. washThe ether phase was washed with water
  4. dry with materialdried (MgSO4)
  5. customthe solvent evaporated under reduced pressure
  6. additionThe resulting oil was mixed with pentane
  7. customto give 3