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2-imidazo[1,5-a]pyridin-1-yl-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid tert-butylamide → N-Tert-Butyl-2-(5,6,7,8-Tetrahydroimidazo[1,5-A]pyridin-1-Yl)-5h-Pyrrolo[2,3-B]pyrazine-7-Carboxamide

HRID 246348
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HRID 246348 반응식
[C:1]([NH:5][C:6]([C:8]1[C:16]2[C:11](=[N:12][CH:13]=[C:14]([C:17]3[N:18]=[CH:19][N:20]4[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=34)[N:15]=2)[N:10](COCC[Si](C)(C)C)[CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(O)(C(F)(F)F)=O.[Pt](=O)=O>[C:1]([NH:5][C:6]([C:8]1[C:16]2[C:11](=[N:12][CH:13]=[C:14]([C:17]3[N:18]=[CH:19][N:20]4[CH2:25][CH2:24][CH2:23][CH2:22][C:21]=34)[N:15]=2)[NH:10][CH:9]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 712796032-imidazo[1,5-a]pyridin-1-yl-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid tert-butylamide

생성물 1

HCID 71280008N-Tert-Butyl-2-(5,6,7,8-Tetrahydroimidazo[1,5-A]pyridin-1-Yl)-5h-Pyrrolo[2,3-B]pyrazine-7-Carboxamide수율 26%

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 6422Trifluoroacetic acid용매

실험 절차

To a solution of 2-imidazo[1,5-a]pyridin-1-yl-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid tert-butylamide (70 mg, 0.15 mmol) in TFA (2 mL) was added platinum(IV) oxide (7 mg, 0.03 mmol). The reaction mixture was stirred under hydrogen (balloon) for 6 h then filtered over Celite, rinsing with CH2Cl2. The filtrate was concentrated. The residue was dissolved in CH2Cl2 (3 mL) and treated with ethylenediamine (0.4 mL). The reaction mixture was stirred for 1 h then quenched with water and extracted with CH2Cl2 (2×). The combined organics were dried over MgSO4 and concentrated. The residue was purified by silica gel chromatography with 0% to 3% MeOH/CH2Cl2 (0.5% NH4OH). The appropriate fractions were combined and concentrated to afford a yellow solid which was triturated with Et2O to obtain 13 mg (26%) of 2-(5,6,7,8-tetrahydro-imidazo[1,5-a]pyridin-1-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid tert-butylamide as a pale yellow solid. MS: (M+H)+=339; 1H NMR (DMSO-d6, 300 MHz): δ (ppm) 12.50 (br. s., 1H), 8.96 (s, 1H), 8.21 (s, 1H), 7.75 (s, 1H), 7.66 (s, 1H), 4.06 (t, J=5.9 Hz, 2H), 3.21 (t, J=6.2 Hz, 2H), 1.76-1.98 (m, 4H), 1.46 (s, 9H).

후처리

  1. filtrationthen filtered over Celite
  2. washrinsing with CH2Cl2
  3. concentrationThe filtrate was concentrated
  4. dissolutionThe residue was dissolved in CH2Cl2 (3 mL)
  5. additiontreated with ethylenediamine (0.4 mL)
  6. stirringThe reaction mixture was stirred for 1 h
  7. customthen quenched with water
  8. extractionextracted with CH2Cl2 (2×)
  9. dry with materialThe combined organics were dried over MgSO4
  10. concentrationconcentrated
  11. customThe residue was purified by silica gel chromatography with 0% to 3% MeOH/CH2Cl2 (0.5% NH4OH)
  12. concentrationconcentrated
  13. customto afford a yellow solid which
  14. customwas triturated with Et2O

출처 및 근거

ORD 기록
ord-432aa5120fd64af98c799dc42ba05eed
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658646B2

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