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Selectfluor → HCID 178526427, 화합물

HRID 520570
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HRID 520570 반응식
[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[N:7][NH:8]2)=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1.[B-](F)(F)(F)[F:15].[B-](F)(F)(F)F.C1[N+]2(CCl)CC[N+](F)(CC2)C1>C(#N)C.C(O)(=O)C>[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([F:15])=[N:7][NH:8]2)=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1
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참가 물질

5

반응물 2

HCID 2724933SelectfluorHCID 247280596-bromo-4-nitro-1H-indazole

생성물 1

HCID 178526427HCID 178526427, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6342Acetonitrile용매

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온도
100 °C

실험 절차

To a solution of 6-bromo-4-nitro-1H-indazole (5 g) in acetonitrile (50 ml) and acetic acid (10 ml) was added Selectfluor (9.39 g). The resulting mixture was heated to 100° C. and stirred for two days. The reaction mixture was concentrated under vacuum. The residue was dissolved in DCM and then filtered off. The sample was absorbed onto silica powder then solid loaded onto the companion where it was purified on a 120 g silica column using a 0-100% ethyl acetate:cyclohexane gradient. The appropriate fractions were combined and concentrated to yield the title compound as an orange solid, 2 g.

후처리

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. dissolutionThe residue was dissolved in DCM
  3. filtrationfiltered off
  4. customThe sample was absorbed onto silica powder
  5. customwas purified on a 120 g silica column
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d3a1492b7bc947e9896a67d40edb8d5d
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09326987B2

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