5-broMo-3-nitrobenzene-1,2-diol synthesis
- Product Name:5-broMo-3-nitrobenzene-1,2-diol
- CAS Number:671779-99-0
- Molecular formula:C6H4BrNO4
- Molecular Weight:234.0043
16634-88-1
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Yield:671779-99-0 98%
Reaction Conditions:
with dihydrogen peroxide;sodium hydroxide in tetrahydrofuran;water at 0 - 20; pH=10 - 11; for 6.5 h;
Steps:
Intermediate D
[000245] To a solution of Compound D2 (40 g, 163 mmol) in THF (260 mL) was added dropwise aq. NaOH solution (0.05 N, 640 mL, 33 mmol) at 0 °C and 30% H202 solution (80 mL). The mixture was stirred for 2 h at rt. The second portion of 30% H202 (80 mL) was added dropwise and the mixture was stirred for 4 h. After cooling to 0 °C, aq. NaOH solution (2 N, 98 mL) was added dropwise until pH10~l 1. The mixture was stirred for 0.5 h and quenched with cone. HC1 at 0 °C until pH 2~3. The mixture was extracted with dichloromethane (250 mL x 3) and washed with brine (300 mL x 2), dried over Na2S04, and concentrated to give Compound D3 (37 g, yield 98%>) as a yellow solid. LC-MS (m/z): 232 [M-l]~; 1H-NMR (CDC13, 400 MHz) major characteristic peaks: δ (ppm) 7.17 (s, 1H), 7.48 (s, 1H), 10.59 (s, 2H).
References:
WO2015/42397,2015,A1 Location in patent:Paragraph 000245
70978-54-0
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1761-61-1
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