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3-Pyridinecarboxaldehyde → HCID 67519540, 화합물

HRID 81929
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HRID 81929 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[C:18]2[C:17]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:11]=[C:10]([NH2:19])[C:9]=2[N:8]=[C:7]1[CH2:20][O:21][CH3:22].[N:23]1[CH:28]=[CH:27][CH:26]=[C:25]([CH:29]=O)[CH:24]=1.C([BH3-])#N.[Na+].C(=O)(O)[O-].[Na+]>C(O)(=O)C.CO>[CH3:22][O:21][CH2:20][C:7]1[N:6]([CH2:5][CH2:4][CH2:3][CH2:2][NH:1][CH2:29][C:25]2[CH:24]=[N:23][CH:28]=[CH:27][CH:26]=2)[C:18]2[C:17]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[N:11]=[C:10]([NH2:19])[C:9]=2[N:8]=1
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참가 물질

7

반응물 4

HCID 103713-PyridinecarboxaldehydeHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydrideHCID 67519397HCID 67519397, 화합물

생성물 1

HCID 67519540HCID 67519540, 화합물수율 15.3%

시약·촉매·용매 2

HCID 176Acetic Acid용매
HCID 887
Methanol
용매

실험 절차

To a round-bottomed flask containing 1-(4-aminobutyl)-2-methoxymethyl-1H-imidazo[4,5-c]quinolin-4-amine (10.0 g, 33.4 mmol) was added methanol (160 mL) followed by acetic acid (40 mL). The reaction was stirred for 5 minutes and pyridine 3-carboxaldehyde (5.4 g, 50.1 mmol) was added and the reaction was stirred overnight at ambient temperature. Sodium cyanoborohydride (1 M in THF, 33.4 mL, 33.4 mmol) was added to the resultant imine in portions over 10 minutes. After 45 minutes the solvent was evaporated to afford an oil. To the oil was added saturated aqueous sodium bicarbonate (200 mL) and the aqueous layer was washed with ethyl acetate (200 mL) and dichloromethane (200 mL). The product was extracted from the aqueous with 20% methanol (2×100 mL) in dichloromethane. The organic layers were combined and the solvent evaporated to afford crude 2-methoxymethyl-1-{4-[(pyridin-3-ylmethyl)amino]butyl}-1H-imidazo[4,5-c]quinolin-4-amine (about 2 g). The aqueous layer was again extracted with 20% dimethylformamide (2×100 mL) in dichloromethane. The organic layers were combined and the solvent evaporated to afford crude 2-methoxymethyl-1-{4-[(pyridin-3-ylmethyl)amino]butyl}-1H-imidazo[4,5-c]quinolin-4-amine (about 2 g).

후처리

  1. stirringthe reaction was stirred overnight at ambient temperature
  2. customAfter 45 minutes the solvent was evaporated
  3. customto afford an oil
  4. washthe aqueous layer was washed with ethyl acetate (200 mL) and dichloromethane (200 mL)
  5. extractionThe product was extracted from the aqueous with 20% methanol (2×100 mL) in dichloromethane
  6. customthe solvent evaporated
  7. customto afford crude 2-methoxymethyl-1-{4-[(pyridin-3-ylmethyl)amino]butyl}-1H-imidazo[4,5-c]quinolin-4-amine (about 2 g)
  8. extractionThe aqueous layer was again extracted with 20% dimethylformamide (2×100 mL) in dichloromethane
  9. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-210821464fab416092c7f551b9388c86
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846710B2

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