Methylamine → 6-(Methylamino)[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one

HRID 1730879노트

반응식

HRID 1730879 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[NH:9][N:10]=2)[N:7]=1.[CH3:12][NH2:13]>C1C=CC=CC=1>[CH3:12][NH:13][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[NH:9][N:10]=2)[N:7]=1

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 64071826-chloro-2H,3H-[1,2,4]triazolo[4,3-b]pyridazin-3-one

생성물 1

HCID 214943106-(Methylamino)[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

20.5 g. of 6-chloro-1,2,4-triazolo[4,3-b]pyridazin-3(2H)-one (0.12 mol.) and a solution of 14.85 g. of methylamine (0.48 mol.) in 160 ml. of benzene are heated in an autoclave at 120° for 5 hours. After cooling, the precipitated product is filtered off and the filtrate is evaporated to dryness. Both portions of 6-methylamino-1,2,4-triazolo[4,3-b]pyridazin-3(2H)-one are treated with dilute aqueous hydrochloric acid, filtered off and recrystallized from water to give 15.8 g. (80%) of material, m.p. > 348° .

후처리

  1. temperatureAfter cooling
  2. filtrationthe precipitated product is filtered off
  3. customthe filtrate is evaporated to dryness
  4. additionBoth portions of 6-methylamino-1,2,4-triazolo[4,3-b]pyridazin-3(2H)-one are treated with dilute aqueous hydrochloric acid
  5. filtrationfiltered off
  6. customrecrystallized from water
  7. customto give 15.8 g

출처 및 근거

ORD 기록
ord-b917996865ba498ba0a6b70eb04a87cc
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03994898

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