Acetic Acid → 6-Chloro-N1-methylbenzene-1,2-diamine

2-Chloro-N-methyl-6-nitrobenzenamine (1.5 g, 8.0 mmol) was dissolved in a mixture of EtOH (15 mL) and H2O (15 ml). Iron powder (2.2 g, 40 mmol) was added followed by Acetic acid (0.55 mL, 9.6 mmol). The reaction was monitored by TLC, after 30 min, the reaction was completed. The reaction mixture was filtered over celite pad and the filtrate was neutralized by saturated NaHCO3 (10 mL). The product was extracted by EtOAc (2*10 mL), the organic layer was washed with brine (10 mL), dried over MgSO4 and concentrated to dryness to afford 920 mg of 6-chloro-N1-methylbenzene-1,2-diamine (Yield: 73%) as dark brown oil.

1. filtrationThe reaction mixture was filtered over celite pad
2. extractionThe product was extracted by EtOAc (2*10 mL)
3. washthe organic layer was washed with brine (10 mL)
4. dry with materialdried over MgSO4
5. concentrationconcentrated to dryness

ORD-Eintrag

ord-a3cf8d726ec54c4f86fd3d9d4d14c4fc

Quelldatensatz

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08674106B2