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Ammonium formate → 1-Piperidinecarboxylic acid, 4-[4-[4-(1H-indazol-3-yl)-1H-1,2,3-triazol-1-yl]phenyl]-, 1,1-dimethylethyl ester

HRID 1520076
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HRID 1520076 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([C:10]2[N:11]=[N:12][N:13]([C:15]3[CH:20]=[CH:19][C:18]([C:21]4[CH2:22][CH2:23][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:25][CH:26]=4)=[CH:17][CH:16]=3)[CH:14]=2)=[N:2]1.C([O-])=O.[NH4+]>C1COCC1.[Pd]>[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([C:10]2[N:11]=[N:12][N:13]([C:15]3[CH:16]=[CH:17][C:18]([CH:21]4[CH2:26][CH2:25][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:23][CH2:22]4)=[CH:19][CH:20]=3)[CH:14]=2)=[N:2]1
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5

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HCID 2723923Ammonium formateHCID 67981119HCID 67981119, 화합물

생성물 1

HCID 679810931-Piperidinecarboxylic acid, 4-[4-[4-(1H-indazol-3-yl)-1H-1,2,3-triazol-1-yl]phenyl]-, 1,1-dimethylethyl ester수율 94.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

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온도
70 °C

실험 절차

In a Parr reactor, Pd/C (10% Pd moistened, 50% water, 24 mg, 0.23 mmol, 0.1 eq.) was suspended in a solution of tert-butyl 4-{4-[4-(1H-indazol-3-yl)-1H-1,2,3-triazol-1-yl]phenyl}-3,6-dihydropyridine-1(2H)-carboxylate (1.0 g; 2.26 mmol; 1.0 eq.) and ammonium formate (2.85 g; 45.2 mmol; 20 eq.) in THF (55 mL). The reaction mixture was stirred for 48 h at 70° C. It was then filtered through a celite pad, the cake was rinsed several times with THF and the filtrate was concentrated to dryness. The resulting residue was partitioned between DCM and water. Organic phase was washed with brine, dried over magnesium sulfate, filtered and concentrated. Purification by flash chromatography on silica (DCM:MeOH, gradient from 100:0 to 95:5) gave the title compound as a white foam (950 mg g; 94.5%). 1H NMR (300 MHz, DMSO-d6) δ 13.36 (brs, 1H), 9.27 (s, 1H), 8.36 (d, J=8.2 Hz, 1H), 8.01-7.93 (m, 2H), 7.61 (d, J=8.4 Hz, 1H), 7.56-7.39 (m, 3H), 7.30-7.20 (m, 1H), 4.27-3.94 (m, 2H), 3.01-2.63 (m, 3H), 1.96-1.70 (m, 2H), 1.69-1.47 (m, 2H), 1.43 (s, 9H). 1H HPLC (max plot) 97.2%; Rt 5.33 min. UPLC/MS: (MS+) 445.2, (MS−) 443.2.

후처리

  1. filtrationIt was then filtered through a celite pad
  2. washthe cake was rinsed several times with THF
  3. concentrationthe filtrate was concentrated to dryness
  4. customThe resulting residue was partitioned between DCM and water
  5. washOrganic phase was washed with brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customPurification by flash chromatography on silica (DCM:MeOH, gradient from 100:0 to 95:5)

출처 및 근거

ORD 기록
ord-1782e6cf51a4461a9da69c3a056a2ef2
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09073892B2

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