4-broMo-3-Methylbenzene-1,2-diaMine synthesis
- Product Name:4-broMo-3-Methylbenzene-1,2-diaMine
- CAS Number:952511-74-9
- Molecular formula:C7H9BrN2
- Molecular Weight:201.06
290353-57-0
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Yield: 91%
Reaction Conditions:
with tin(II) chloride dihdyrate in ethanol;ethyl acetate at 80; for 12 h;
Steps:
18.2
step 2: A mixture of 154 (40 g,154 mmol), SnCl2-2H20 (208 g, 920 mmol), EtOAc (300 mL) and EtOH (150 mL) was heated to 80 °C for 12 h, cooled to RT, poured into crushed ice (2 Kg) and the pH adjusted to pH 7-8 with solid NaHCC>3. The solid was filtered and washed with EtOAc. The filtrate was thrice extracted with EtOAc. The combined extracts were washed with brine, dried (Na2SO (), filtered and concentrated in vacuo. The crude product was purified by Si02 chromatography eluting with an EtOAc/hexane gradient (10 to 50% EtOAc) to afford 28 g (91%) of 4-bromo-3 -methyl- 1,2- benzenediamine (156) as a brown oil: MS (ESI) m/z = 202 [M+l]+.
References:
F. HOFFMANN-LA ROCHE AG;ALIAGAS-MARTIN, Ignacio;CRAWFORD, James;LEE, Wendy;MATHIEU, Simon;RUDOLPH, Joachim WO2013/26914, 2013, A1 Location in patent:Page/Page column 143
854624-54-7
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570-24-1
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55289-36-6
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1325729-87-0
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