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Azobisisobutyronitrile → 5-(Bromomethyl)-4-chloropyrrolo[2,1-f][1,2,4]triazine

HRID 347523
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HRID 347523 반응식
[Cl:1][C:2]1[C:7]2=[C:8]([CH3:11])[CH:9]=[CH:10][N:6]2[N:5]=[CH:4][N:3]=1.CC(N=NC(C#N)(C)C)(C#N)C.C1C(=O)N([Br:31])C(=O)C1>C(Cl)(Cl)(Cl)Cl>[Br:31][CH2:11][C:8]1[CH:9]=[CH:10][N:6]2[C:7]=1[C:2]([Cl:1])=[N:3][CH:4]=[N:5]2
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참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 218742274-Chloro-5-methylpyrrolo(2,1-f)(1,2,4)triazine

생성물 1

HCID 218743865-(Bromomethyl)-4-chloropyrrolo[2,1-f][1,2,4]triazine수율 92%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

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온도
100 °C

실험 절차

A mixture of 4-chloro-5-methyl-pyrrolo[2,1-f][1,2,4]triazine (2.0 g, 11.93 mmol, WO 03/042172) and AIBN (195 mg, 1.19 mmol) in CCl4 (80 mL) under N2 was heated to 100° C. for 5 min, NBS (2.55 g, 14.3 mmol) was added. The reaction mixture was stirred for 10 min, then cooled to rt, filtered. The CCl4 layer was washed with dilute NaHCO3 aqueous solution, dried (MgSO4), filtered and concentrated to give the desired product (2.70 g, 92%).

후처리

  1. temperaturecooled to rt
  2. filtrationfiltered
  3. washThe CCl4 layer was washed with dilute NaHCO3 aqueous solution
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f6683d8730884417b890543c1cf3e495
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07173031B2

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