反应 #640527
ord-dde274e722b0409d87706d81630193ab
反应方程式
4-(1H-benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine
4-(1H-Benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine
LiAlH4
THF
THF
→
title compound
4-(1H-Benzimidazol-2-yl)-furazan-3-yl-N-(3-hydroxypropyl)-amine
反应物
试剂
无
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他is quenched by careful addition of aqueous saturated solution of sodium sulphate
- 2过滤The suspension is filtered
- 3其他the filtrate evaporated to dryness
- 4其他Crystallization
- 5workup.ADDITIONby addition of hexane
实验过程
A solution of 4-(1H-benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine (0.272 g, 0.947 mmol, Example 6a) in THF (5 ml) is added dropwise at 0° C. to an efficiently stirred suspension of LiAlH4 (0.054 g, 1.42 mmol) in THF (5 ml). After stirring for 16 hours at room temperature the mixture is quenched by careful addition of aqueous saturated solution of sodium sulphate. The suspension is filtered and the filtrate evaporated to dryness. Crystallization by addition of hexane yields the title compound in pure form. 1H-NMR (400 MHz, d6-DMSO): 13.6 (s, 1H); 7.66 (m, 2H); 7.31 (m, 2H); 6.92 (t, 1H); 4.61 (m, 1H); 3.51 (m, 2H); 3.39 (m, 2H); 1.81 (m, 2H).