HRID1796002

反应详情

EQUATION

反应方程式

HRID 1796002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-benzyl-5-chloro-4-oxo-3,4-dihydro-pyrrolo[2,1-f][1,2,4]triazine-2-carbaldehyde (Example 22 E, 50 mg, 0.17 mmol) in EtOH (1 mL) was added 4 A molecular sieves (50 mg), (3-amino-propyl)-carbamic acid tert-butyl ester (Fluka, 33 mg, 0.19 mmol) and NaBH(OAc)3 (55 mg, 0.26 mmol) under Ar. The reaction mixture was stirred at rt for 2 h, filtered and the filtrate was concentrated in vacuo. The residue was purified by flash column chromatography (SiO2, 1–2% MeOH/CHCl3) to afford the desired compound, as a colorless oil (12 mg, 16%): MS (ESI+) 446 (M++H).

WORKUP

后处理

  1. filtrationfiltered
  2. concentrationthe filtrate was concentrated in vacuo
  3. customThe residue was purified by flash column chromatography (SiO2, 1–2% MeOH/CHCl3)