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Acetic Acid → 1-Benzyl-4-[N-ethyl-N-(6-fluoro-3-(isopropylamino)-2-pyridinyl)amino]piperidine

HRID 361854
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HRID 361854 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH2:25][CH3:26])[C:15]2[C:20]([N+:21]([O-])=O)=[CH:19][CH:18]=[C:17]([F:24])[N:16]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:27](N1CCC(N(CC)C2C(N)=CC=C(F)N=2)CC1)[C:28]1C=CC=C[CH:29]=1.CC(C)=O.C(O)(=O)C.C([BH3-])#N.[Na+].C(=O)(O)[O-].[Na+]>C(O)C.CO.[Pt]=O>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH2:25][CH3:26])[C:15]2[C:20]([NH:21][CH:28]([CH3:29])[CH3:27])=[CH:19][CH:18]=[C:17]([F:24])[N:16]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 6

HCID 176Acetic AcidHCID 180AcetoneHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydrideHCID 105945621-Benzyl-4-[N-ethyl-N-(6-fluoro-3-nitro-2-pyridyl)amino]piperidineHCID 106162651-benzyl-4-[N-ethyl-N-(6-fluoro-3-(amino)-2-pyridinyl)amino]piperidine

생성물 1

HCID 10571219
1-Benzyl-4-[N-ethyl-N-(6-fluoro-3-(isopropylamino)-2-pyridinyl)amino]piperidine

시약·촉매·용매 3

HCID 82844Platinum oxide (PtO)촉매HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

1-Benzyl-4-[N-ethyl-N-(6-fluoro-3-(nitro)-2-pyridinyl)amino]piperidine (EXAMPLE 195, 3.0 g, 8.37 mmol) is dissolved in ethanol (500 ml) and 0.75 g of platinum oxide is added. The reaction is placed on a Parr hydrogenator at 10 psi for 1 hr and then filtered through diatomaceous earth and concentrated under reduced pressure. The crude 1-benzyl-4-[N-ethyl-N-(6-fluoro-3-(amino)-2-pyridinyl)amino]piperidine (3.0 g, 9.13 mmol) is immediately dissolved in methanol (18 ml) and acetone (0.74 ml, 10.04 mmol) and acetic acid (13.1 ml, 228.3 mmol) are added. The reaction is stirred for 10 min, then cooled to 0° and sodium cyanoborohydride (0.61 g, 9.7 mmol) is added. The reaction is slowly warmed to 20°-25° and stirred for 18 hr. Then solid sodium bicarbonate is added with caution and the reaction is extracted with chloroform, washed with saline, dried over sodium sulfate and concentrated under reduced pressure. Purification via flash column chromatography (5% ethyl acetate/hexane to 10% ethyl acetate/hexane) gives the title compound, NMR (300 MHz, CDCl3) 7.26-7.15, 6.88, 6.49, 4.28, 3.40, 3.44, 3.04, 2.93, 2.82, 1.93, 1.72-1.52, 1.13 and 0.81δ; CMR (CDCl3, 75 MHz) 155.9, 152.5, 146.1, 138.0, 129.1, 128.1, 126.9, 121.8, 104.3, 62.9, 57.5, 52.7, 44.4, 41.2, 29.7 and 22.8δ.

후처리

  1. filtrationfiltered through diatomaceous earth
  2. concentrationconcentrated under reduced pressure
  3. temperaturecooled to 0°
  4. temperatureThe reaction is slowly warmed to 20°-25°
  5. stirringstirred for 18 hr
  6. extractionthe reaction is extracted with chloroform
  7. washwashed with saline
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customPurification via flash column chromatography (5% ethyl acetate/hexane to 10% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-e9cd92ef2bf94896943f58dd815e063b
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05866589

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