HRID1698067

反应详情

EQUATION

反应方程式

HRID 1698067 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl 4-[5-(6-nitro-1,3-benzothiazol-2-yl)pyridin-2-yl]piperazine-1-carboxylate (90 mg, 0.2 mmol) was dissolved in methanol (8 mL). After addition of 7M NH3 in methanol (2 mL), palladium on carbon (10%, 10 mg) was added and the flask was evacuated and filled with hydrogen gas. The reaction mixture was shaken under an atmosphere of hydrogen overnight. The mixture was thereafter filtered through diatomaceous earth and evaporated in vacuo. The crude product was purified by flash column chromatography (heptane:ethyl acetate; 70:30 to 35:65), to give the title compound (38 mg) as a solid. MS m/z (M+H) 412.

WORKUP

后处理

  1. additionwas added
  2. customthe flask was evacuated
  3. additionfilled with hydrogen gas
  4. filtrationThe mixture was thereafter filtered through diatomaceous earth
  5. customevaporated in vacuo
  6. customThe crude product was purified by flash column chromatography (heptane:ethyl acetate; 70:30 to 35:65)