反应详情

Combine 4-(5-formyl-thiophen-2-yloxy)-benzamide (99 mg, 0.40 mmol) from Example 1 part B, method B, with 3-methyl-butylamine (0.056 mL, 0.48 mmol), methyl orthoformate (0.53 mL) and methanol (0.8 mL). Stir the resulting mixture for 3 hours and then add sodium borohydride in portions. Let stir for few hours. Then, concentrate to remove the methanol. Partition the resulting residue between H2O (4 mL) and CH2Cl2 (6 ml). Dry the organic layer over sodium sulfate, filter and concentrate. Purify through flash chromatography [CH2Cl2/Ammonia (2.0 M in methanol) 20/1] to provide the title compound.

1. stirringLet stir for few hours
2. concentrationThen, concentrate
3. customto remove the methanol
4. customPartition the resulting residue between H2O (4 mL) and CH2Cl2 (6 ml)
5. dry with materialDry the organic layer over sodium sulfate
6. filtrationfilter
7. concentrationconcentrate
8. customPurify through flash chromatography [CH2Cl2/Ammonia (2.0 M in methanol) 20/1]