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Piperazine → N-sec-butyl-5-(4-(2-fluorophenyl)-1H-imidazol-5-yl)thiazolo[5,4-b]pyridin-2-amine

HRID 1452981
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HRID 1452981 반응식
[CH:1]([NH:5][C:6]1[S:7][C:8]2[C:13]([N:14]=1)=[CH:12][CH:11]=[C:10]([CH:15]=O)[N:9]=2)([CH2:3][CH3:4])[CH3:2].[NH4+].[OH-].[F:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH:26]([N+:37]#[C-:38])S(C1C=CC(C)=CC=1)(=O)=O.[NH:39]1CCNCC1>C1COCC1.CCOC(C)=O>[CH:1]([NH:5][C:6]1[S:7][C:8]2[C:13]([N:14]=1)=[CH:12][CH:11]=[C:10]([C:15]1[NH:39][CH:38]=[N:37][C:26]=1[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=1[F:19])[N:9]=2)([CH2:3][CH3:4])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 4837PiperazineHCID 14923Ammonium HydroxideHCID 467382311-Fluoro-2-(isocyano(tosyl)methyl)benzeneHCID 575272422-(Sec-butylamino)thiazolo[5,4-b]pyridine-5-carbaldehyde

생성물 1

HCID 15986167N-sec-butyl-5-(4-(2-fluorophenyl)-1H-imidazol-5-yl)thiazolo[5,4-b]pyridin-2-amine수율 26%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 8857Ethyl Acetate용매

실험 절차

A solution of 2-(sec-butylamino)thiazolo[5,4-b]pyridine-5-carbaldehyde (presumed 0.24 mmol, 1.0 eq.) and concentrated aqueous NH4OH (0.050 mL) in THF (0.8 mL) was stirred overnight. 1-Fluoro-2-(isocyano(tosyl)methyl)benzene (0.0841 g, 0.291 mmol, 1.2 eq.) and piperazine (0.0394 g, 0.457 mmol, 1.9 eq.) were added, and the reaction mixture was stirred overnight. It was then diluted with EtOAc and washed with water, saturated aqueous NaHCO3, and brine, dried over Na2SO4, filtered, and concentrated in vacuo. MeOH was added to the residue, and the mixture was subjected to autoprep. The appropriate fractions were collected, and NaHCO3 (s) was added. The solution was then concentrated in vacuo not to dryness and extracted with CH2Cl2 (3×). The organic layers were combined, dried over Na2SO4, filtered, and concentrated in vacuo to give N-sec-butyl-5-(4-(2-fluorophenyl)-1H-imidazol-5-yl)thiazolo[5,4-b]pyridin-2-amine as a yellow solid (0.0228 g, 26% yield). LC/MS (MH)=368.23.

후처리

  1. washwashed with water, saturated aqueous NaHCO3, and brine
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. additionMeOH was added to the residue
  6. customThe appropriate fractions were collected
  7. additionNaHCO3 (s) was added
  8. concentrationThe solution was then concentrated in vacuo not to dryness
  9. extractionextracted with CH2Cl2 (3×)
  10. dry with materialdried over Na2SO4
  11. filtrationfiltered
  12. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-fcaeeb2d481f490c886903533dd9eb1f
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07473784B2

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