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2-Benzofurancarboxaldehyde → HCID 68575168, 화합물

HRID 2111922
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HRID 2111922 반응식
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[C:15]([O:19][C:20]([N:22]1[CH2:27][CH2:26][CH:25]([NH:28][CH2:29][CH2:30][CH:31]([CH3:33])[CH3:32])[CH2:24][CH2:23]1)=[O:21])([CH3:18])([CH3:17])[CH3:16].[O:34]1[C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=2[CH:36]=[C:35]1[CH:43]=O.C([O-])(O)=O.[Na+]>ClCCl>[C:15]([O:19][C:20]([N:22]1[CH2:23][CH2:24][CH:25]([N:28]([CH2:43][C:35]2[O:34][C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=3[CH:36]=2)[CH2:29][CH2:30][CH:31]([CH3:33])[CH3:32])[CH2:26][CH2:27]1)=[O:21])([CH3:18])([CH3:17])[CH3:16]
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참가 물질

6

반응물 4

HCID 613412-BenzofurancarboxaldehydeHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 43652145HCID 43652145, 화합물

생성물 1

HCID 68575168HCID 68575168, 화합물수율 105.4%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

실험 절차

Sodium triacetoxyborohydride (0.88 g, 4.16 mmol) is added to a stirred solution of 4-(3-methyl-butylamino)-piperidine-1-carboxylic acid tert-butyl ester (0.75 g, 2.77 mmol), benzofuran-2-carboxaldehyde (0.50 g, 3.46 mmol), and dichloromethane (14 ml). The reaction is stirred overnight at room temperature under nitrogen. The reaction is poured into aqueous saturated NaHCO3 (50 ml) and extracted with dichloromethane (25 ml×3). The organic layer is washed with aqueous saturated NaHCO3 and dried over Na2SO4, and filtered. The crude product is concentrated on a rotary evaporator and purified by flash chromatography on silica gel eluting with 0-30% (1:2 (10% NH4OH in methanol):ethanol) to yield (1.17 g) of 4-{[(benzofuran-2-yl)methyl]-(3-methylbutyl)-amino}-piperidine-1-carboxylic acid tert-butyl ester: mass spectrum (ion spray): m/z=401 (M+1); 1H NMR (CDCl3): δ=7.57-7.41 (2H, m), 7.30-7.16 (2H, m), 6.55 (1H, s), 4.15 (2H, brs), 3.81 (2H, s), 2.75-2.56 (6H, m), 1.80 (2H, brd), 1.63-1.53 (3H, m), 1.46 (9H, s), 1.42-1.33 (1H, m), 0.92-0.85 (6H, m).

후처리

  1. extractionextracted with dichloromethane (25 ml×3)
  2. washThe organic layer is washed with aqueous saturated NaHCO3
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationThe crude product is concentrated on a rotary evaporator
  6. custompurified by flash chromatography on silica gel eluting with 0-30% (1:2 (10% NH4OH in methanol):ethanol)

출처 및 근거

ORD 기록
ord-6e0c4636e2544f7c9137b0c59baf6d62
출처 데이터셋
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07521462B2

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