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Methanol → 3-[1-(4-Acetylamino-benzyl)-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl)-propionic acid methyl ester

HRID 2240600
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HRID 2240600 반응식
[CH3:1][O:2][C:3](=[O:21])[CH2:4][CH2:5][C:6]1[C:7](=[O:20])[N:8]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][CH:14]=2)[CH2:9][CH2:10][CH:11]=1.O(OC(C)=O)[O:23][C:24]([CH3:26])=O.C(N(CC)CC)C.CO>C(Cl)Cl.CN(C1C=CN=CC=1)C>[CH3:1][O:2][C:3](=[O:21])[CH2:4][CH2:5][C:6]1[C:7](=[O:20])[N:8]([CH2:12][C:13]2[CH:14]=[CH:15][C:16]([NH:19][C:24](=[O:23])[CH3:26])=[CH:17][CH:18]=2)[CH2:9][CH2:10][CH:11]=1
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7

반응물 4

HCID 887MethanolHCID 8471TriethylamineHCID 19362196Acetate oxygenHCID 574434273-[1-(4-Amino-benzyl)-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl]-propionic acid methyl ester

생성물 1

HCID 574434283-[1-(4-Acetylamino-benzyl)-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl)-propionic acid methyl ester수율 44%

시약·촉매·용매 2

HCID 14284
4-(Dimethylamino)pyridine
촉매
HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

17.5 mg of 3-[1-(4-amino-benzyl)-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl]-propionic acid methyl ester (h) prepared by above Step 1 was dissolved in methylene chloride solution (0.06 mM). And then 6 μl of (AcO)2O (0.07 mM), 0.01 ml of triethylamine (0.08 mM) and 1.0 mg of DMAP (0.008 mM) were added thereto and the mixture was stirred for 3 hrs at 0° C. The reaction was stopped by adding methanol and the mixture was extracted three times with 10 ml of ethyl acetate. The organic layer was washed with saturated NaCl solution, dried over anhydrous MgSO4, filtered and concentrated in vacuo. The resulting compound was purified with Silica gel column chromatography with ethylacetate as an eluant to give 46 mg of 3-[1-(4-acetylamino-benzyl)-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl)-propionic acid methyl ester (i) (yield: 44%).

후처리

  1. extractionthe mixture was extracted three times with 10 ml of ethyl acetate
  2. washThe organic layer was washed with saturated NaCl solution
  3. dry with materialdried over anhydrous MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe resulting compound was purified with Silica gel column chromatography with ethylacetate as an eluant

출처 및 근거

ORD 기록
ord-cff8dbc8988a4c019549db026386126f
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07723376B2

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