Реакция #417977

ord-4b207866bef24aa2bdebbf6b53031d8c

Уравнение реакции

CC(=O)O
acetic acid
O
water
O
water
COC(=O)c1cccc(-c2noc(C)n2)c1
methyl 3-(5-methyl-1,2,4-oxadiazol-3-yl)benzoate
CC(=O)O.COC(=O)c1cccc(C(=N)N)c1
methyl 3-carbamimidoylbenzoate acetate

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеis hydrogenated at room temperature
  2. 2
    ФильтрацияThe catalyst is filtered off
  3. 3
    Другоеthe filtrate is evaporated
  4. 4
    Температураheated to the boil
  5. 5
    Фильтрацияfiltered off with suction
  6. 6
    ДругоеThe residue is dried in vacuo
  7. 7
    Другое=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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08877751B2uspto-grants-2014_11