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ChemicalBook CAS DataBase List Methyl carbazate

Methyl carbazate synthesis

5synthesis methods
Methylcarbazate can be used as pharmaceutical intermediates and biochemical reagents, mainly in laboratory research and development processes. Its synthesis method is as follows:A mixture of dimethyl carbonate and hydrazine hydrate was heated to 50 °C, stirred for 30 min, and then stirred at room temperature for 24 h. Water, methanol, and excess dimethyl carbonate were distilled off under reduced pressure. 
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Yield:6294-89-9 94%

Reaction Conditions:

with hydrazine hydrate at 20 - 50; for 24.5 h;

Steps:

Preparation of methyl hydrazinecarboxylate (2)
A mixture of dimethyl carbonate (1, 45.0 g, 0.50 mol) and hydrazine hydrate (29.4 mL, 0.48 mol) was added into a 250 mL round-bottom flask equipped with a condenser. The reaction mixture was heated to 50 °C, stirred for 30 min, and then stirred at room temperature for 24 h. Water, methanol, and excess dimethyl carbonate were distilled off under reduced pressure. After dryness, a white crystal (2) (42.3 g) was obtained with a yield of 94%, mp 69-70 °C.1H NMR (300 MHz, CDCl3): δ 3.73 (s, 3H, CH3-O), 3.77 (d, 2H,J=1.85Hz, -NH2), 6.09 (s, 1H, -NH).

References:

Zhang, Jing-Peng;Qin, Yao-Guo;Dong, Ya-Wen;Song, Dun-Lun;Duan, Hong-Xia;Yang, Xin-Ling [Chinese Chemical Letters,2017,vol. 28,# 2,p. 372 - 376] Location in patent:supporting information

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