4-METHYL-3-NITROBENZOHYDRAZIDE synthesis
- Product Name:4-METHYL-3-NITROBENZOHYDRAZIDE
- CAS Number:19013-12-8
- Molecular formula:C8H9N3O3
- Molecular Weight:195.18
796070-73-0
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Yield:19013-12-8 99%
Reaction Conditions:
Stage #1: C13H17N3O5with trifluoroacetic acid at 0 - 20; for 1 h;
Stage #2: with sodium carbonate in water;ethyl acetate;
Steps:
68.B
68A (4.4g, 15 mmol) as a solid was added in portions to trifluoroacetic acid (45 mL) at 0°C, and the mixture was stirred at this temperature for 30 min and at rt for an additional 30 minutes. The mixture was then concentrated in vacuo and the resulting white solid was partitioned between 2N aq sodium carbonate (200 mL) and EtOAc (200 mL). The layers were separated and the aqueous portion was extracted with additional EtOAc (5 x 100 mL), and the combined extracts were washed with brine (100 mL), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to yield 2.96g (99%) of 68B as a white solid. HPLC tR = 1. 05 min. 1H NMR (500 MHz, d6-DMSO) : 8 10.20 (br s, 1H), 8.42 (s, 1H), 8.05 (d, 1H), 7.62 (d, 1H), 5.43 (br s, 2H), 2.56 (s, 3H). LCMS [M+H] + = 196.3
References:
WO2005/42537,2005,A1 Location in patent:Page/Page column 83
94-08-6
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