反应详情

To a solution of [3-[4-(3-Amino-propyl)-piperazin-1-yl]-propyl]-(1H-benzimidazol-2-yl)-amine (Intermediate of example 44) (130 mg, 0.41 mmol) in CH2Cl2 (4 mL) isobutyraldehyde (62 μL, 0.46 mmol), triethylamine (26 μL, 0.16 mmol) and 3 Å molecular sieves are added. The reaction media is stirred for 3 h and cooled before NaBH4 (78 mg, 2.05 mmol) is added portionwise over 30 min. Stirring is left for 1.5 h, water (10 mL) is added and the media is filtered. Compound is extracted with CH2Cl2 (3×20 mL). Combined organic layers are dried over MgSO4. Crude compound is purified by thick-layer chromatography (CH2Cl2/MeOH/NH4OH: 90/10/1.2).

1. customThe reaction media
2. additionis added portionwise over 30 min
3. stirringStirring
4. waitis left for 1.5 h
5. filtrationthe media is filtered
6. extractionCompound is extracted with CH2Cl2 (3×20 mL)
7. dry with materialCombined organic layers are dried over MgSO4
8. customCrude compound is purified by thick-layer chromatography (CH2Cl2/MeOH/NH4OH: 90/10/1.2)