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Ether hydrochloride → 2-tert-Butyl-N-methyl-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazol-5-amine

HRID 1987193
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HRID 1987193 반응식
[C:1]([C:5]1[N:9]([CH2:10][CH:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[C:8]2[CH:17]=[CH:18][C:19]([NH:21][C:22](=O)OC)=[CH:20][C:7]=2[N:6]=1)([CH3:4])([CH3:3])[CH3:2].Cl.CCOCC.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[C:1]([C:5]1[N:9]([CH2:10][CH:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[C:8]2[CH:17]=[CH:18][C:19]([NH:21][CH3:22])=[CH:20][C:7]=2[N:6]=1)([CH3:4])([CH3:2])[CH3:3]
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참가 물질

5

반응물 3

HCID 10953452Ether hydrochlorideHCID 21226445Aluminium lithium hydrideHCID 57723208Methyl [2-tert-butyl-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazol-5-yl]carbamate

생성물 1

HCID 574410762-tert-Butyl-N-methyl-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazol-5-amine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

Methyl [2-tert-butyl-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazol-5-yl]carbamate (1.80 g, 5.21 mmol) was dissolved in 75 mL of THF at 0° C. 1M HCl/ether (7.3 mL, 7.29 mmol) was added dropwise and the solution was stirred at 0° C. for 15 min. LiAlH4 (988 mg, 26.1 mmol) was added slowly and the solution was stirred at rt overnight. The reaction was quenched at 0° C. by the addition of MeOH (5 mL) followed by water (10 mL) and the solution was left to stir at rt for 30 min. Anhydrous Na2SO4 (10 g) was added and the solution was stirred at rt for another 30 min. The solution was filtered and the solvent was evaporated. The residue was dissolved in EtOAc and washed with aqueous NaHCO3 solution, brine and dried over anhydrous MgSO4. The solvent was evaporated. Yield: 1.54 g (98%). 1H NMR (400 MHz, CHLOROFORM-D) δ 1.49-1.53 (m, 4 H), 1.53-1.57 (m, 9 H), 2.22-2.32 (m, 1 H), 2.87 (s, 3 H), 3.26-3.35 (m, 2 H), 3.95 (t, J=3.03 Hz, 1 H), 3.97-4.00 (m, 1 H), 4.13 (d, J=7.42 Hz, 2 H), 6.61 (dd, J=8.59, 2.15 Hz, 1 H), 6.99 (d, J=1.95 Hz, 1 H), 7.11 (d, J=8.59 Hz, 1 H).

후처리

  1. stirringthe solution was stirred at rt overnight
  2. customThe reaction was quenched at 0° C. by the addition of MeOH (5 mL)
  3. waitthe solution was left
  4. stirringto stir at rt for 30 min
  5. additionAnhydrous Na2SO4 (10 g) was added
  6. stirringthe solution was stirred at rt for another 30 min
  7. filtrationThe solution was filtered
  8. customthe solvent was evaporated
  9. dissolutionThe residue was dissolved in EtOAc
  10. washwashed with aqueous NaHCO3 solution, brine
  11. dry with materialdried over anhydrous MgSO4
  12. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-1bf59fb178b948e7a3d67b381b32e091
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07550495B2

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