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Trimethylsilylacetylene → tert-butyl 3-((trimethylsilyl)ethynyl)-1H-indazole-1-carboxylate

HRID 1520001
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HRID 1520001 반응식
I[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[N:3]=1.[CH3:18][Si:19]([C:22]#[CH:23])([CH3:21])[CH3:20]>C(Cl)Cl.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:18][Si:19]([C:22]#[C:23][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[N:3]=1)([CH3:21])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 66111TrimethylsilylacetyleneHCID 11473390tert-butyl 3-iodo-1H-indazole-1-carboxylate

생성물 1

HCID 67981125tert-butyl 3-((trimethylsilyl)ethynyl)-1H-indazole-1-carboxylate수율 69%

시약·촉매·용매 2

HCID 178418476HCID 178418476, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

A mixture of tert-butyl 3-iodo-1H-indazole-1-carboxylate (prepared as described in J. Med. Chem. (2008), 51(12), 3460-3465); (34 g; 99 mmol; 1.00 eq.), (trimethylsilyl)acetylene (16.6 mL; 119 mmol; 1.20 eq.), PdCl2(PPh3)2 (2.77 g; 3.95 mmol; 0.04 eq.) and TEA (41 mL) was heated overnight at 50° C. The reaction mixture was then diluted with DCM and washed three times with an aqueous saturated solution of NH4Cl. Organic layer was dried over magnesium sulfate, filtered and concentrated. This crude was solubilized in DCM and the precipitate obtained was removed by filtration through a celite pad. Purification by flash chromatography on silica (Heptane/EtOAc; gradient from 98:2 to 2:98) afforded the title compound as a beige solid (20 g, 69% yield). 1H NMR (300 MHz, DMSO-d6) δ: 8.12 (d, J=8.5 Hz, 1H), 7.78 (d, J=8.5 Hz, 1H), 7.70 (m, 1H), 7.46 (m, 1H), 1.65 (s, 9H), 0.32 (s, 9H).

후처리

  1. washwashed three times with an aqueous saturated solution of NH4Cl
  2. dry with materialOrganic layer was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customthe precipitate obtained
  6. customwas removed by filtration through a celite pad
  7. customPurification by flash chromatography on silica (Heptane/EtOAc; gradient from 98:2 to 2:98)

출처 및 근거

ORD 기록
ord-103a7ddb5c5245d8851f98e9831ea4ad
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09073892B2

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