반응 #1951116

ord-7c66aa33cfc743a6a46ae284730bdea5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A white precipitate separated during the addition
  2. 2
    기타the solid was collected on a filter
  3. 3
    기타The solid was then collected on
  4. 4
    여과a filter
  5. 5
    세척washed with some additional concentrated ammonium hydroxide
  6. 6
    기타After drying

실험 절차

A solution of 155 mg (1 mmol) of 5-chloro[1,2,4]triazolo[1,5-c]pyrimidine [D. J. Brown and K. Shinozuka, Aust. J. Chem., 33, 1147 (1980)] in 6 mL of dry ethanol was added gradually to a vigorously stirred solution of 198 mg (204 mg, 4 mmol) of hydrazine monohydrate in 2 mL of dry ethanol. A white precipitate separated during the addition. After 1.5 h, the solid was collected on a filter. It was suspended in 2 mL of concentrated ammonium hydroxide and agitated for a few minutes. The solid was then collected on a filter and washed with some additional concentrated ammonium hydroxide, then with some ethanol, and finally with a large volume of diethyl ether. After drying, the title compound was obtained as a white solid, mp 245-246° C. (decomposition). LC-MS 151 (M+1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07625888B2uspto-grants-2009_12