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Triethylsilane → HCID 13285353, 화합물

HRID 1593515
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반응식

HRID 1593515 반응식
[Cl:1][CH2:2][C:3]([C:5]1[C:13]2[C:8](=[N:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH:6]=1)=O.C([SiH](CC)CC)C>C(O)(C(F)(F)F)=O.CCOC(C)=O.C(=O)([O-])[O-].[Na+].[Na+]>[Cl:1][CH2:2][CH2:3][C:5]1[C:13]2[C:8](=[N:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH:6]=1
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참가 물질

6

반응물 2

HCID 12052TriethylsilaneHCID 127782172-Chloro-1-(1H-pyrrolo[2,3-b]pyridin-3-yl)ethan-1-one

생성물 1

HCID 13285353HCID 13285353, 화합물

시약·촉매·용매 3

HCID 6422Trifluoroacetic acid용매HCID 8857Ethyl Acetate용매HCID 10340Sodium Carbonate용매

실험 절차

A stirred solution of 2-chloro-1-(1H-pyrrolo[2,3-b]pyridin-3-yl)ethanone (12.5 g) in TFA at room temperature is treated with triethylsilane (72 mL, 7 eq.), stirred for 16 h, diluted with EtOAc and saturated sodium carbonate to pH 8. The phases are separated and the organic phase is dried over MgSO4 and concentrated in vacuo. The resultant residue is purified by flash chromatography (silica gel, 10% EtOAc in ether as eluent) to give the title pyrrolo[2,3-b]pyridine compound, identified by NMR and mass spectral analyses.

후처리

  1. customThe phases are separated
  2. dry with materialthe organic phase is dried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customThe resultant residue is purified by flash chromatography (silica gel, 10% EtOAc in ether as eluent)

출처 및 근거

ORD 기록
ord-e7eded962bbd4a0bb25952179cbb735c
출처 데이터셋
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07297705B2

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