Bromine → 4-Bromo-6-phenylpyridazin-3-amine

HRID 1755307노트

반응식

HRID 1755307 반응식
[C:1]1([C:7]2[N:12]=[N:11][C:10]([NH2:13])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])(O)=O.[Na+].[Br:19]Br>CO>[Br:19][C:9]1[CH:8]=[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[N:12]=[N:11][C:10]=1[NH2:13]

참가 물질

5

반응물 3

HCID 24408BromineHCID 516892Sodium BicarbonateHCID 119589156-Phenylpyridazin-3-amine

생성물 1

HCID 583863604-Bromo-6-phenylpyridazin-3-amine수율 33.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In a 150 mL round bottom flask was placed 6-phenylpyridazin-3-amine (2.5 g, 14.5 mmol), NaHCO3 (2.44 g, 29 mmol) and methanol (50 mL) then to this suspension was added Br2 (2.317 g, 14.5 mmol) drop wise over about 30 minutes at room temperature. The mixture was stirred for 16 h, then filtered and concentrated in vacuo. The residue was purified by chromatography (silica gel, 200-300 mesh, petroleum ether:ethyl acetate=2:1) to give 4-bromo-6-phenylpyridazin-3-amine (1.2 g, 33%) as a light orange solid. LC-MS: [M+H]+, 250.0, tR=1.487 min.

후처리

  1. customIn a 150 mL round bottom flask was placed
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by chromatography (silica gel, 200-300 mesh, petroleum ether:ethyl acetate=2:1)

출처 및 근거

ORD 기록
ord-dc69f5c8911d47afb49c0a67735122db
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169259B2

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