HRID53179

反应详情

EQUATION

反应方程式

HRID 53179 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of 14.1 g (47.7 mmol, 1.00 eq.) of t-butyl 4-(acetoxymethyl)-3-nitrobenzoate in MeOH (200 mL) was added 27.0 mL (477 mmol, 10.0 eq.) of hydrazine hydrate (55% hydrazine). The resulting yellow solution was stirred at 25° C. for 4 hr. EtOAc (250 mL) and saturated aq. NaCl (85 mL) were added, and the organic layer collected after shaking. The organic layer was washed further with saturated aq. NaCl (2×85 mL), and then dried (MgSO4). Removal of volatiles in vacuo gave the product in 93% yield as yellow crystals. The reaction is represented in Scheme 5.

WORKUP

后处理

  1. customthe organic layer collected
  2. stirringafter shaking
  3. washThe organic layer was washed further with saturated aq. NaCl (2×85 mL)
  4. dry with materialdried (MgSO4)
  5. customRemoval of volatiles in vacuo
  6. customgave the product in 93% yield as yellow crystals