Реакция #417977
ord-4b207866bef24aa2bdebbf6b53031d8c
Уравнение реакции
acetic acid
water
water
methyl 3-(5-methyl-1,2,4-oxadiazol-3-yl)benzoate
→
methyl 3-carbamimidoylbenzoate acetate
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Другоеis hydrogenated at room temperature
- 2ФильтрацияThe catalyst is filtered off
- 3Другоеthe filtrate is evaporated
- 4Температураheated to the boil
- 5Фильтрацияfiltered off with suction
- 6ДругоеThe residue is dried in vacuo
- 7Другое=1.40 min (method A)
Методика
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).