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Ozone → 4-[2-(4-tert-Butyl-phenyl)-3H-imidazo[4,5-c]pyridin-7-yl]-piperazine-1-carboxylic acid benzyl ester

HRID 729355
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HRID 729355 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH:14]=[CH:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O=[O+][O-].P(OCC)(OCC)OCC.[C:29]([C:33]1[CH:38]=[CH:37][C:36]([C:39]2[NH:40][C:41]3[C:46]([NH2:47])=[CH:45][N:44]=[CH:43][C:42]=3[N:48]=2)=[CH:35][CH:34]=1)([CH3:32])([CH3:31])[CH3:30].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C(Cl)Cl.CO>[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH2:14][N:47]([C:46]2[C:41]3[N:40]=[C:39]([C:36]4[CH:37]=[CH:38][C:33]([C:29]([CH3:32])([CH3:31])[CH3:30])=[CH:34][CH:35]=4)[NH:48][C:42]=3[CH:43]=[N:44][CH:45]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

8

반응물 5

HCID 24823OzoneHCID 31215Triethyl phosphiteHCID 643471Benzyl 3-pyrroline-1-carboxylateHCID 5049666Sodium triacetoxyborohydrideHCID 178440764HCID 178440764, 화합물

생성물 1

HCID 578327604-[2-(4-tert-Butyl-phenyl)-3H-imidazo[4,5-c]pyridin-7-yl]-piperazine-1-carboxylic acid benzyl ester
수율 2.5%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

반응 조건

온도
-78 °C

실험 절차

2,5-Dihydro-pyrrole-1-carboxylic acid benzyl ester 6 was dissolved in DCM (5 ml) and MeOH (2 ml). It was cooled to −78° C. and treated with ozone until it was blue in color. Triethyl phosphite (246 mg, 1.48 mmol) was added and the solution was allowed to stir for 5 minutes. 2-(4-tert-Butyl-phenyl)-1H-imidazo[4,5-c] pyridin-7-ylamine 4 (266 mg, 1.00 mmol) was added followed by sodium triacetoxyborohydride (538 mg, 2.54 mmol). This mixture was allowed to stir for 18 hours. Mass spectroscopy showed no starting material left after this time, and the solvent was removed under vacuum. The crude was taken up in ethyl acetate and washed with a saturated sodium bicarbonate solution, brine, dried over MgSO4, and the crude was purified by HPLC (Method E), yielding the title product 7 (12 mg (2.5%), 0.026 mmol). 1H NMR (DMSO-d6): δ 8.88 (bs, 1H), 8.23 (d, J=8.5 Hz, 2H), 7.96 (s, 1H), 7.68 (d, J=8.5 Hz, 2H), 7.38 (m, 5H), 5.15 (s, 2H), 1.33 (s, 9H). MS (ESI-POS): [M+H]+=470; MS(ESI-NEG):[M−H]−=468.

후처리

  1. stirringto stir for 18 hours
  2. waitleft after this time
  3. customthe solvent was removed under vacuum
  4. washwashed with a saturated sodium bicarbonate solution, brine
  5. dry with materialdried over MgSO4
  6. customthe crude was purified by HPLC (Method E)

출처 및 근거

ORD 기록
ord-ad390ac47f0c4b5e9dc6f68d48e90946
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582634B2

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