2,5-DIMETHOXYBENZENESULFONOHYDRAZIDE synthesis
- Product Name:2,5-DIMETHOXYBENZENESULFONOHYDRAZIDE
- CAS Number:19116-91-7
- Molecular formula:C8H12N2O4S
- Molecular Weight:232.26
1483-28-9
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Yield:19116-91-7 78%
Reaction Conditions:
with hydrazine hydrate in tetrahydrofuran at 0 - 20;
Steps:
8 4.1.2.8
2,5-Dimethoxybenzenesulfonohydrazide (5p)
General procedure: To solution of 1 mmol of arylsulfonyl chloride 4i-w in 10 ml of THF, 1.1 mmol of hydrazine-hydrate in 10 ml THF were added drop wise at 0-5 8C with stirring. After stirring 1-2 h at rt 20 ml of water were added, the precipitate was filtered, dried and crystallized from benzene or hexane. HPLC analysis revealed single peaks for all tested compounds. Yield 78%, m.p. 98-100 °C. 1H NMR (DMSO-d6): δ 3.82 (s, 3H, CH3O), 3.90 (s, 3H, CH3O), 7.22 (m, 2H, HAr), 7.31 (d, 1H, JHH = 2.6 Hz, HAr), 7.74 (s, 1H, NH). EI-MS (m/z): 233 [M+1]+. Anal. calcd. for C8H12N2O4S: C, 41.37; H, 5.21; N, 12.06; O, 27.55; S, 13.81; found: C, 41.52; H, 5.38; N, 12.29.
References:
Luzina, Elena L.;Popov, Anatoliy V. [Journal of Fluorine Chemistry,2013,vol. 148,p. 41 - 48]
150-78-7
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