HRID251223

反应详情

EQUATION

反应方程式

HRID 251223 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N1-(3-methyl-pyridin-2-yl)-N1-(5,6,7,8-tetrahydro-quinolin-8-yl)-propane-1,3-diamine (63 mg, 0.20 mmol) and (tert-butoxycarbonylimino-pyrazol-1-yl-methyl)-carbamic acid tert-butyl ester (110 mg, 0.31 mmol) was stirred in THF (0.3 mL) for 16 hours. The solvent was removed under reduced pressure, CH2Cl2 (10 mL) was added and the organic phase washed with 15% aqueous NaOH solution (5×5 mL). The organic phase was then dried (Na2SO4) and concentrated under reduced pressure to afford, after column chromatography with silica gel (33:1:0.1 CH2Cl2/MeOH:NH4OH), ({3-[(3-methyl-pyridin-2-ylmethyl)-(5,6,7,8-tetrahydro-quinolin-8-yl)-amino]-propyl}-tert-butoxycarbonylimino-methyl)-carbamic acid tert butyl ester as a pale brown sticky solid (50 mg, 49%),

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure, CH2Cl2 (10 mL)
  2. additionwas added
  3. washthe organic phase washed with 15% aqueous NaOH solution (5×5 mL)
  4. dry with materialThe organic phase was then dried (Na2SO4)
  5. concentrationconcentrated under reduced pressure
  6. customto afford