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ChemicalBook CAS DataBase List Methyl carbazate
6294-89-9

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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