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Acetic Acid → 6-(Methyloxy)-7-nitro-2-(1-propyl-4-piperidinyl)-1,2,3,4-tetrahydroisoquinoline

HRID 1014310
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HRID 1014310 반응식
[CH2:1]([N:4]1[CH2:9][CH2:8][C:7](=O)[CH2:6][CH2:5]1)[CH2:2][CH3:3].[CH3:11][O:12][C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][C:22]=1[N+:23]([O-:25])=[O:24])[CH2:19][NH:18][CH2:17][CH2:16]2.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCCl.C(N(CC)CC)C>[CH3:11][O:12][C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][C:22]=1[N+:23]([O-:25])=[O:24])[CH2:19][N:18]([CH:7]1[CH2:8][CH2:9][N:4]([CH2:1][CH2:2][CH3:3])[CH2:5][CH2:6]1)[CH2:17][CH2:16]2
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참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 900061-Propyl-4-piperidoneHCID 5049666Sodium triacetoxyborohydrideHCID 594418746-Methoxy-7-nitro-1,2,3,4-tetrahydroisoquinoline

생성물 1

HCID 594416526-(Methyloxy)-7-nitro-2-(1-propyl-4-piperidinyl)-1,2,3,4-tetrahydroisoquinoline수율 89.4%

시약·촉매·용매 2

HCID 11
1,2-Dichloroethane
용매
HCID 8471Triethylamine용매

실험 절차

A mixture of 1-propyl-4-piperidinone (01.25 mL, 8.3 mmol), 6-(methyloxy)-7-nitro-1,2,3,4-tetrahydroisoquinoline (1.0 g, 4.8 mmol), acetic acid (0.55 mL) and triethylamine (1.3 mL) in 1,2-dichloroethane (5 mL) was stirred for 30 minutes. Sodium triacetoxyborohydride (1.8 g, 2.8 mmol) was added. After stirring for 12 hours the reaction was quenched by the addition of saturated NaHCO3 (aq). The reaction was diluted with dichloromethane and the layers were separated. The aqueous phase was extracted with dichloromethane. The combined organic layers were washed with water, dried over MgSO4 and concentrated onto silica gel. The crude material was purified by flash column chromatography to give 6-(methyloxy)-7-nitro-2-(1-propyl-4-piperidinyl)-1,2,3,4-tetrahydroisoquinoline (1.43 g, 89%). 1H NMR (400 MHz, CDCl3) δ ppm 7.60 (s, 1 H), 6.78 (s, 1 H), 3.91 (s, 3 H), 3.73 (s, 2 H), 3.07 (d, J=9.17 Hz, 2 H), 2.91 (t, J=5.87 Hz, 2 H), 2.83 (t, J=5.68 Hz 2 H), 2.47-2.60 (m, 1 H), 2.29-2.42 (m, 2 H), 2.04 (d, J=10.63 Hz, 2 H), 1.68-1.94 (m, 4 H), 1.49-1.66 (m, 2 H), 0.91 (t, J=7.33 Hz, 3 H).

후처리

  1. stirringAfter stirring for 12 hours the reaction
  2. customwas quenched by the addition of saturated NaHCO3 (aq)
  3. additionThe reaction was diluted with dichloromethane
  4. customthe layers were separated
  5. extractionThe aqueous phase was extracted with dichloromethane
  6. washThe combined organic layers were washed with water
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated onto silica gel
  9. customThe crude material was purified by flash column chromatography

출처 및 근거

ORD 기록
ord-40026031d9024d30a50a24d62fc4f167
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981903B2

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