反应 #417977

反应方程式

acetic acid

water

water

methyl 3-(5-methyl-1,2,4-oxadiazol-3-yl)benzoate

→

methyl 3-carbamimidoylbenzoate acetate

溶剂

methanol

反应条件

后处理

1. 1
   其他is hydrogenated at room temperature
2. 2
   过滤The catalyst is filtered off
3. 3
   其他the filtrate is evaporated
4. 4
   温度heated to the boil
5. 5
   过滤filtered off with suction
6. 6
   其他The residue is dried in vacuo
7. 7
   其他=1.40 min (method A)

实验过程

150 ml of acetic acid, 150 ml of water and 50 g of water-moist Raney nickel are added to a solution of 327 g (1.47 mol) of methyl 3-(5-methyl-1,2,4-oxadiazol-3-yl)benzoate in 3 l of methanol, and the mixture is hydrogenated at room temperature and atmospheric pressure for 18 hours. The catalyst is filtered off, and the filtrate is evaporated. The residue is taken up in tert-butyl methyl ether, heated to the boil and filtered off with suction. The residue is dried in vacuo: 3-methoxycarbonylbenzamidinium acetate as colourless crystals; m.p. 222°; ESI 179 (M+H); HPLC: Rt.=1.40 min (method A).

来源